|
1
|
Embarez DH, Razek ASA, Basalious EB, Mahmoud M, Hamdy NM. Acetaminophen-traces bioremediation with novel phenotypically and genotypically characterized 2 Streptomyces strains using chemo-informatics, in vivo, and in vitro experiments for cytotoxicity and biological activity. J Genet Eng Biotechnol 2023; 21:171. [PMID: 38112983 PMCID: PMC10730784 DOI: 10.1186/s43141-023-00602-w] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Abstract] [Key Words] [Grants] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 07/14/2023] [Accepted: 11/14/2023] [Indexed: 12/21/2023]
Abstract
We isolated two novel bacterial strains, active against the environmental pollutant acetaminophen/Paracetamol®. Streptomyces chrestomyceticus (symbol RS2) and Flavofuscus (symbol M33) collected from El-Natrun Valley, Egypt-water, sediment, and sand samples, taxonomically characterized using a transmission electron microscope (TEM). Genotypic identification, based on 16S rRNA gene sequence analysis followed by BLAST alignment, were deposited on the NCBI as 2 novel strains https://www.ncbi.nlm.nih.gov/nuccore/OM665324 and https://www.ncbi.nlm.nih.gov/nuccore/OM665325 . The phylogenetic tree was constructed. Acetaminophen secondary or intermediate product's chemical structure was identified by GC/LC MS. Some selected acetaminophen secondary-product extracts and derived compounds were examined against a panel of test micro-organisms and fortunately showed a good anti-microbial effect. In silico chemo-informatics Swiss ADMET evaluation was used in the selected bio-degradation extracts for absorption (gastric), distribution (to CNS), metabolism (hepatic), excretion (renal), and finally not toxic, being non-mutagenic/teratogenic or genotoxic, virtually. Moreover, in vitro cytotoxic activity of these selected bio-degradation secondary products was examined against HepG2 and MCF7 cancer cell lines, where M33 and RS2 extract effects on acetaminophen/paracetamol bio-degradation products were safe, with higher IC50 on HepG2 and MCF7 than the acetaminophen/paracetamol IC50 of 108.5 μg/ml. Moreover, an in vivo oral acute single-dose toxicity experiment was conducted, to confirm these in vitro and in silico lower toxicity (better safety) than acetaminophen/paracetamol.
Collapse
Affiliation(s)
- Donia H Embarez
- Biochemistry Department, Faculty of Science, Ain Shams University, Cairo, 11566, Abassia, Egypt
| | - Ahmed S Abdel Razek
- Microbial Chemistry Department, Genetic Engineering and Biotechnology Research Division, National Research Centre, Giza, 12622, Dokki, Egypt
| | - Emad B Basalious
- Department of Pharmaceutics and Industrial Pharmacy, Faculty of Pharmacy, Cairo University, Cairo, 11562, Al Kasr El-Aini, Egypt
| | - Magdi Mahmoud
- Biochemistry Department, Faculty of Science, Ain Shams University, Cairo, 11566, Abassia, Egypt
| | - Nadia M Hamdy
- Department of Biochemistry, Faculty of Pharmacy, Ain Shams University, Cairo, 11566, Abassia, Egypt.
| |
Collapse
|
|
2
|
Mohamed HM, Saad AS, Morsi AM, Essam HM. Green RP-HPLC method for simultaneous determination of sofosbuvir, ledipasvir, velpatasvir antivirals and beyond in their bulk material and co-formulated products. Microchem J 2022. [DOI: 10.1016/j.microc.2022.108344] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 12/24/2022]
|
|
3
|
Vaishnavi A. Sarangdhar, Ramanlal N. Kachave. Overview of UHPLC-MS: an Effective and Sensitive Hyphenated Technique. JOURNAL OF ANALYTICAL CHEMISTRY 2022. [DOI: 10.1134/s1061934822110119] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Track Full Text] [Subscribe] [Scholar Register] [Indexed: 11/13/2022]
|
|
4
|
Heidari H, Hassan-Zadeh Z, Khoubnasabjafari M. Ultrasensitive fluorometric determination of daclatasvir in exhaled breath condensate samples after magnetic solid-phase extraction by carbon-coated Fe3O4 magnetic nanoparticles: method optimization via central composite design combined with desirability function. CHEMICAL PAPERS 2022. [DOI: 10.1007/s11696-022-02346-2] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Track Full Text] [Subscribe] [Scholar Register] [Indexed: 11/28/2022]
|
|
5
|
Keyvan K, Sohrabi MR, Motiee F. An intelligent method based on feed-forward artificial neural network and least square support vector machine for the simultaneous spectrophotometric estimation of anti hepatitis C virus drugs in pharmaceutical formulation and biological fluid. SPECTROCHIMICA ACTA. PART A, MOLECULAR AND BIOMOLECULAR SPECTROSCOPY 2021; 263:120190. [PMID: 34332240 DOI: 10.1016/j.saa.2021.120190] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Track Full Text] [Subscribe] [Scholar Register] [Received: 04/04/2021] [Revised: 06/23/2021] [Accepted: 07/13/2021] [Indexed: 06/13/2023]
Abstract
This study proposed simple and reliable spectrophotometry method for simultaneous analysis of hepatitis C antiviral binary mixture containing sofosbuvir (SOF) and daclatasvir (DAC). This technique is based on the use of feed-forward artificial neural network (FF-ANN) and least square support vector machine (LS-SVM). FF-NN with Levenberg-Marquardt (LM) and Cartesian genetic programming (CGP) algorithms was trained to determine the best number of hidden layers and the number of neurons. This comparison demonstrated that the LM algorithm had the minimum mean square error (MSE) for SOF (1.59 × 10-28) and DAC (4.71 × 10-28). In LS-SVM model, the optimum regularization parameter (γ) and width of the function (σ) were achieved with root mean square error (RMSE) of 0.9355 and 0.2641 for SOF and DAC, respectively. The coefficient of determination (R2) value of mixtures containing SOF and DAC was 0.996 and 0.997, respectively. The percentage recovery values were in the range of 94.03-104.58 and 94.04-106.41 for SOF and DAC, respectively. Statistical test (ANOVA) was implemented to compare high-performance liquid chromatography (HPLC) and spectrophotometry, which showed no significant difference. These results indicate that the proposed method possesses great potential ability for prediction of concentration of components in pharmaceutical formulations.
Collapse
Affiliation(s)
- Kiarash Keyvan
- Department of Chemistry, North Tehran Branch, Islamic Azad University, Tehran, Iran
| | - Mahmoud Reza Sohrabi
- Department of Chemistry, North Tehran Branch, Islamic Azad University, Tehran, Iran.
| | - Fereshteh Motiee
- Department of Chemistry, North Tehran Branch, Islamic Azad University, Tehran, Iran
| |
Collapse
|
|
6
|
El-Yazbi AF, Elashkar NE, Ahmed HM, Talaat W, Abdel-Hay KM. Cost-effective green chromatographic method for the simultaneous determination of four commonly used direct-acting antiviral drugs in plasma and various pharmaceutical formulations. Microchem J 2021. [DOI: 10.1016/j.microc.2021.106512] [Citation(s) in RCA: 2] [Impact Index Per Article: 0.5] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 02/07/2023]
|
|
7
|
Fayed AS, Hegazy MA, Kamel EB, Eissa MS. HPLC-UV and TLC-Densitometry Methods for Simultaneous Determination of Sofosbuvir and Daclatasvir: Application to Darvoni® Tablet. J Chromatogr Sci 2021; 60:606-612. [PMID: 34355234 DOI: 10.1093/chromsci/bmab100] [Citation(s) in RCA: 1] [Impact Index Per Article: 0.3] [Reference Citation Analysis] [Abstract] [Journal Information] [Subscribe] [Scholar Register] [Received: 05/26/2021] [Accepted: 07/18/2021] [Indexed: 11/13/2022]
Abstract
Sofosbuvir and daclatasvir are co-formulated as directly acting antiviral agents used for treatment of hepatitis C virus. Two chromatographic methods were developed for their determination; the first one is an Reversed phase-high performance liquid chromatography (RP-HPLC) method, in which the separation was performed on C8 Zorbax® SB column (4.6 × 250 mm, 5 μm) using acetonitrile:water:0.05 M phosphate buffer, pH = 8 (50:45:5, v/v/v) as a mobile phase, and ultraviolet detection was performed at 280 nm. Good resolution was obtained, and linearity was confirmed in the range of 10-100 μg/mL for both drugs. The second method is Thin layer chromatography (TLC)-densitometric one, in which sofosbuvir and daclatasvir were separated on silica gel plates using ethyl acetate:hexane:methanol (9:0.5:0.5, v/v/v) as a developing system and the scanning wavelength was 280 nm. Linearity was confirmed over a concentration range of 0.4-25.4 μg/band for sofosbuvir, whereas for daclatasvir linearity scanning was in the range of 0.4-12.8 μg/band. Both antiviral agents can be quantified simultaneously in one analytical run, which is a great time- and cost-saving valor of the developed methods. This valor is even more important in the case of the combined dosage form (Darvoni® tablets) to the pharmaceutical market.
Collapse
Affiliation(s)
- Ahmed S Fayed
- Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr-El Aini Street, 11562 Cairo, Egypt
| | - Maha A Hegazy
- Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr-El Aini Street, 11562 Cairo, Egypt
| | - Ebraam B Kamel
- Pharmaceutical Chemistry Department, Faculty of Pharmacy, Egyptian Russian University, Badr City, 11829 Cairo, Egypt
| | - Maya S Eissa
- Pharmaceutical Chemistry Department, Faculty of Pharmacy, Egyptian Russian University, Badr City, 11829 Cairo, Egypt
| |
Collapse
|
|
8
|
Çelebier M. Ultrafiltration-based Sample Preparation for Pharmaceutical Analysis. CURR PHARM ANAL 2021. [DOI: 10.2174/1573412916999200729172653] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/22/2022]
Abstract
Pharmaceutical analysis plays an important role in all steps of drug development processes.
Analysis of active pharmaceutical ingredients in biological samples needs sample preparation techniques
to prevent the signal of the analyte from interferences coming from matrix components. Ultrafiltration
is a well-known technique used in the food and pharmaceutical industry. Commercial ultrafiltration
devices have been frequently used on proteomics and metabolomics studies for sample preparation.
In pharmaceutical analysis, these devices have been employed to analyze the free concentration of
drugs in biological fluids after filtration. However, they have been rarely used to determine the total
concentration of targeted compounds when it is compared with some other common sample preparation
techniques. Ultrafiltration-based sample preparation might be used to clean-up the sample easily
from matrix components especially on bioanalysis performed with high-performance liquid chromatography
(HPLC). In the case of using protein precipitation agents on filtration procedure, the quantitative
recovery of this non-selective unique technique is competitive with solid-phase extraction.
Collapse
Affiliation(s)
- Mustafa Çelebier
- Department of Analytical Chemistry, Faculty of Pharmacy, Hacettepe University, Ankara, Turkey
| |
Collapse
|
|
9
|
Ezzeldin E, Abo-Talib NF, Tammam MH, Asiri YA, Amr AEGE, Almehizia AA. Validated Reversed-Phase Liquid Chromatographic Method with Gradient Elution for Simultaneous Determination of the Antiviral Agents: Sofosbuvir, Ledipasvir, Daclatasvir, and Simeprevir in Their Dosage Forms. Molecules 2020; 25:molecules25204611. [PMID: 33050433 PMCID: PMC7587186 DOI: 10.3390/molecules25204611] [Citation(s) in RCA: 1] [Impact Index Per Article: 0.2] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Download PDF] [Figures] [Journal Information] [Subscribe] [Scholar Register] [Received: 08/18/2020] [Revised: 09/25/2020] [Accepted: 09/29/2020] [Indexed: 12/18/2022] Open
Abstract
A simple, rapid, sensitive, and precise reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of four direct-acting antivirals, sofosbuvir (SF), ledipasvir (LD), declatasvir (DC), and simeprevir (SM), in their respective pharmaceutical formulations. Effective chromatographic separation was achieved on an Agilent Eclipse plus C8 column (250 mm × 4.6 mm, 5 µm) at 40 °C with gradient elution using a mobile phase composed of acetonitrile:phosphate buffer (pH 6.5). The quantification of SF and DC was based on peak area measurements at 260 nm, while the quantification of LD and SM was achieved at 330 nm. The linearity was acceptable from 1.0 to 20.0 μg/mL for the studied drugs, with correlation coefficients >0.999. The analytical performance of the newly proposed HPLC procedure was thoroughly validated according to ICH guidelines in terms of linearity, precision (RSD%, 0.39-1.57), accuracy (98.05-101.90%), specificity, limit of detection (LOD) (0.022-0.039 μg/mL), limit of quantification (LOQ) (0.067-0.118 μg/mL), and robustness. The validated HPLC method was successfully used to analyze the abovementioned drugs in their pure and dosage forms without interference from common excipients present in commercial formulations.
Collapse
Affiliation(s)
- Essam Ezzeldin
- Pharmaceutical Chemistry Department, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia; (E.E.); (A.E.-G.E.A.); (A.A.A.)
- Bioavailability Center, National Organization for Drug Control and Research (NODCAR), Giza P.O. Box 29, Egypt
| | - Nisreen F. Abo-Talib
- Bioavailability Center, National Organization for Drug Control and Research (NODCAR), Giza P.O. Box 29, Egypt
- Correspondence: (N.F.A.-T.); (M.H.T.)
| | - Marwa H. Tammam
- Bioavailability Center, National Organization for Drug Control and Research (NODCAR), Giza P.O. Box 29, Egypt
- Correspondence: (N.F.A.-T.); (M.H.T.)
| | - Yousif A. Asiri
- Clinical Pharmacy Department, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia;
| | - Abd El-Galil E. Amr
- Pharmaceutical Chemistry Department, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia; (E.E.); (A.E.-G.E.A.); (A.A.A.)
- Applied Organic Chemistry Department, National Research Center, Dokki, Cairo 12622, Egypt
| | - Abdulrahman A. Almehizia
- Pharmaceutical Chemistry Department, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia; (E.E.); (A.E.-G.E.A.); (A.A.A.)
| |
Collapse
|
|
10
|
Liu S, Yang L, Wang S, Pan J. Simultaneous Determination of 9 Main Components of Lonicera japonica Thunb. by UPLC-MS/MS and Analysed Combine With Chemometrics. Nat Prod Commun 2020. [DOI: 10.1177/1934578x20953272] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/16/2022] Open
Abstract
The purpose of this article is to establish a method to use ultra-high performance liquid chromatography (UPLC)-mass spectrometry (MS)/MS to simultaneously determine 9 main components of Lonicera japonica Thunb. in negative-ion scanning mode, and the main components were analyzed by chemometrics. The chromatographic separation uses the Thermo Hypersil GOLD column (100 mm × 2.1 mm, 1.9 µm) with a constant temperature of 45 °C. The mobile phase consists of methanol and water containing 0.2% formic acid. The results show that 9 compounds had a good linear relationship ( R² > 0.9991), and both intraday and interday precisions and stability have the eligible ranges of relative SDs (RSDs; 0.96%-2.26%, 0.52%-3.04%, and 0.85%-2.15%, respectively). The recovery rates were between 75.90% and 110.58%. The results of chemometrics including hierarchical cluster analysis and principal component analysis showed that there were obvious differences in the content of active components in L. japonica from different regions, and the compounds with the highest contribution to the drug were identified. Through the UPLC-MS/MS combined chemometrics analysis of L. japonica, this experiment can provide a reference for further research on the modernization and innovation of L. japonica and the application research of a high level and multidirection.
Collapse
Affiliation(s)
- Songtao Liu
- Heilongjiang University of Chinese Medicine, Harbin, China
| | - Lin Yang
- Heilongjiang University of Chinese Medicine, Harbin, China
- School of Pharmacy, Jiangxi University of traditional Chinese Medicine, Jiangxi, China
| | - Song Wang
- Heilongjiang University of Chinese Medicine, Harbin, China
| | - Junying Pan
- Heilongjiang University of Chinese Medicine, Harbin, China
| |
Collapse
|
|
11
|
El-badawy FM, Mohamed MA, El-Desoky HS. Fabrication of an electrochemical sensor based on manganese oxide nanoparticles supported on reduced graphene oxide for determination of subnanomolar level of anti-hepatitis C daclatasvir in the formulation and biological models. Microchem J 2020. [DOI: 10.1016/j.microc.2020.104914] [Citation(s) in RCA: 17] [Impact Index Per Article: 3.4] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 02/03/2023]
|
|
12
|
Compensate for or Minimize Matrix Effects? Strategies for Overcoming Matrix Effects in Liquid Chromatography-Mass Spectrometry Technique: A Tutorial Review. Molecules 2020; 25:molecules25133047. [PMID: 32635301 PMCID: PMC7412464 DOI: 10.3390/molecules25133047] [Citation(s) in RCA: 115] [Impact Index Per Article: 23.0] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Download PDF] [Figures] [Journal Information] [Subscribe] [Scholar Register] [Received: 06/15/2020] [Revised: 06/30/2020] [Accepted: 07/01/2020] [Indexed: 11/16/2022] Open
Abstract
In recent decades, mass spectrometry techniques, particularly when combined with separation methods such as high-performance liquid chromatography, have become increasingly important in pharmaceutical, bio-analytical, environmental, and food science applications because they afford high selectivity and sensitivity. However, mass spectrometry has limitations due to the matrix effects (ME), which can be particularly marked in complex mixes, when the analyte co-elutes together with other molecules, altering analysis results quantitatively. This may be detrimental during method validation, negatively affecting reproducibility, linearity, selectivity, accuracy, and sensitivity. Starting from literature and own experience, this review intends to provide a simple guideline for selecting the best operative conditions to overcome matrix effects in LC-MS techniques, to obtain the best result in the shortest time. The proposed methodology can be of benefit in different sectors, such as pharmaceutical, bio-analytical, environmental, and food sciences. Depending on the required sensitivity, analysts may minimize or compensate for ME. When sensitivity is crucial, analysis must try to minimize ME by adjusting MS parameters, chromatographic conditions, or optimizing clean-up. On the contrary, to compensate for ME analysts should have recourse to calibration approaches depending on the availability of blank matrix. When blank matrices are available, calibration can occur through isotope labeled internal standards and matrix matched calibration standards; conversely, when blank matrices are not available, calibration can be performed through isotope labeled internal standards, background subtraction, or surrogate matrices. In any case, an adjusting of MS parameters, chromatographic conditions, or a clean-up are necessary.
Collapse
|
|
13
|
Elkhoudary MM, Selim BM, AbdelSalam RA, Hadad GM, El-Gindy A. Development and validation of a simple HPTLC method for the determination of new hepatitis C subtype 4 antiviral agents in their tablet dosage form. JPC-J PLANAR CHROMAT 2020. [DOI: 10.1007/s00764-019-00006-y] [Citation(s) in RCA: 4] [Impact Index Per Article: 0.8] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 12/26/2022]
|
|
14
|
Optimization of a liquid chromatography method for the analysis of related substances in daclatasvir tablets using design of experiments integrated with the steepest ascent method and Monte Carlo simulation. J Pharm Biomed Anal 2020; 178:112943. [PMID: 31677954 DOI: 10.1016/j.jpba.2019.112943] [Citation(s) in RCA: 3] [Impact Index Per Article: 0.6] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 05/14/2019] [Revised: 10/17/2019] [Accepted: 10/17/2019] [Indexed: 11/20/2022]
Abstract
Analytical method for the determination of related substances (RS) in Daclatasvir tablets was optimised using quality by design (QbD) approach. Seven degradants (each more than 1.0%) generated during oxidation study, adversely affected the selectivity of the method. Coelution of the degradant peaks with API and known impurities, suggested failure in developing a stability indicating method. To overcome the shortcomings and develop a robust method, QbD principles were incorporated. Resolution was the critical quality attribute (CQA) and buffer pH, column oven temperature, gradient slope and flow rate were the critical method variables (CMVs) studied through design of experiments (DoE). Discovery of an unknown impurity (named as impurity D, about1.0%) was a key finding from this DoE study. The most crucial responses viz. Resolution between impurity D and the main peak and resolution between the main peak and impurity E demanded contradictory pH requirements. To select the right pH, responses were prioritised and eventually to attain the desired resolution between Daclatasvir and impurity E the value for pH was fixed to 3.0. Next, to improve resolution between impurity D and Daclatasvir, method of steepest ascent was applied to locate an apt value for column oven temperature. Accordingly, experiments were performed at different temperatures along the path of rapid increase in response. Finally, at 45 °C (pH :3.0), both the critical pairs were well resolved. The global optimum was determined through a Response surface methodology (RSM) design with pH and column oven temperature as critical factors. pH 3.0, column oven temperature 44 °C, % MP. B 45% and flow rate 1.0 mL min-1 was found to be the optimum condition. Further, the design space was complimented by establishment of a robust zone through Monte Carlo simulation and capability analysis. An analytical control strategy (ACS) was set up to ensure that the method repeatedly meets its acceptance criteria. The optimised method was successfully validated within the factor ranges mentioned in the ACS. Despite various intricacies, the QbD approach facilitated systematic optimisation of a stability indicating robust method.
Collapse
|
|
15
|
Ultra-high performance liquid chromatography-MS/MS (UHPLC-MS/MS) in practice: analysis of drugs and pharmaceutical formulations. FUTURE JOURNAL OF PHARMACEUTICAL SCIENCES 2019. [DOI: 10.1186/s43094-019-0007-8] [Citation(s) in RCA: 13] [Impact Index Per Article: 2.2] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 12/12/2022] Open
Abstract
Abstract
Background
UHPLC-MS/MS is connected in various research facilities for the qualitative and quantitative investigation of a pharmaceutical substance, pharmaceutical items, and biological specimen.
Main body
The commence review article is an endeavor to offer pervasive awareness around assorted aspects and details about the UHPLC-MS/MS and related techniques with the aim on practice to an estimation of medicinal active agents in the last 10 years. The article also focused on isolation, separation, and characterization of present impurity in drug and biological samples.
Conclusion
Review article compiles a general overview of medicinally important drugs and their analysis with UHPLC-MS/MS. It gives fundamental thought regarding applications of UHPLC-MS/MS for the study on safety limit. The summary of developed UHPLC-MS/MS methods gives a contribution to the future trend and limitations in this area of research.
Collapse
|
|
16
|
Youssef AA, Magdy N, Hussein LA, El-Kosasy AM. Validated RP-HPLC Method for Simultaneous Determination of Ribavirin, Sofosbuvir and Daclatasvir in Human Plasma: A Treatment Protocol Administered to HCV Patients in Egypt. J Chromatogr Sci 2019; 57:636-643. [PMID: 31063182 DOI: 10.1093/chromsci/bmz038] [Citation(s) in RCA: 11] [Impact Index Per Article: 1.8] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 11/01/2018] [Revised: 03/11/2019] [Accepted: 04/05/2019] [Indexed: 02/06/2023]
Abstract
Egypt has the highest prevalence of hepatitis C virus (HCV) in the world thus it launched a national program for eliminating HCV aiming to treat 300,000 HCV patients per year. Three anti-HCV co-administered drugs; ribavirin (RBV), sofosbuvir (SF) daclatasvir (DAC) were simultaneously determined in human plasma by a validated, simple and sensitive RP-HPLC method using propyl paraben as an internal standard. Liquid-liquid extraction using ethyl acetate was used for samples extraction. Chromatographic separation was achieved on Scharlau® C18 column (250 × 4.6 mm2, 5 μm). Gradient elution was employed with a mobile phase mixture of water and acetonitrile at a flow rate 1 mL/min. UV detection using photodiode array detector was carried out at 207, 260 and 312 nm for RBV, SF and DAC, respectively. Method validation was performed according to the FDA guidelines for bioanalytical method validation. The calibration curves were linear over the ranges (0.5-80, 0.1-40 and 0.5-80 μg/mL) with average recoveries (100.64-108.28%, 98.48-105.91% and 97.68-101.38%) for RBV, SF and DAC, respectively. The intra-day and inter-day precision and accuracy results were within the acceptable limits. Stability assays revealed that the three studied analytes were stable during sample storage, preparation and injection. The method can be successfully applied in routine analysis of plasma of HCV patients treated with this combination therapy which aids in therapeutic drug monitoring and patients' follow-up especially in Egypt and other developing countries fighting HCV.
Collapse
Affiliation(s)
- Aya A Youssef
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Organization of African Unity Street, Abassia, Cairo, Egypt
| | - N Magdy
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Organization of African Unity Street, Abassia, Cairo, Egypt
| | - Lobna A Hussein
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Organization of African Unity Street, Abassia, Cairo, Egypt
| | - A M El-Kosasy
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Organization of African Unity Street, Abassia, Cairo, Egypt
| |
Collapse
|
|
17
|
Simultaneous analysis of daclatasvir with its three organic impurities: Application in stability studies, pharmaceuticals and serum samples. Microchem J 2019. [DOI: 10.1016/j.microc.2019.03.045] [Citation(s) in RCA: 4] [Impact Index Per Article: 0.7] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/20/2022]
|
|
18
|
Azab SM. A comprehensive structural comparison between cellulose and starch polymers functionalized cobalt nanoparticles sensors for the nanomolar detection of paracetamol. J Electroanal Chem (Lausanne) 2019. [DOI: 10.1016/j.jelechem.2019.04.011] [Citation(s) in RCA: 14] [Impact Index Per Article: 2.3] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/16/2022]
|
|
19
|
Zidan DW, Hassan WS, ElMasry MS, Shalaby AA. Novel spectrophotometric and factor-based multivariate calibration-prediction techniques for determination of two inhibitors of hepatitis C-virus and hepatocellular carcinoma in pure, human urine, and human plasma. SPECTROCHIMICA ACTA. PART A, MOLECULAR AND BIOMOLECULAR SPECTROSCOPY 2019; 213:288-300. [PMID: 30708286 DOI: 10.1016/j.saa.2018.12.052] [Citation(s) in RCA: 3] [Impact Index Per Article: 0.5] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Track Full Text] [Subscribe] [Scholar Register] [Received: 10/30/2018] [Revised: 12/20/2018] [Accepted: 12/29/2018] [Indexed: 06/09/2023]
Abstract
Novel univariate and multivariate factor-based calibration-prediction techniques were validated for simultaneous ultraviolet spectrophotometric determination of ribavirin (RIV), daclatasvir (DAV), sofosbuvir (SOV), and sorafenib (SON) which are co-administered for treatment of hepatocellular carcinoma (HCC) that results from Hepatitis C-virus (HCV) infection in their commercial products and in biological fluids. Determination of these compounds is essential owing to their pharmacotherapeutic benefits. Due to spectral overlapping of RIV, DAV, SOV, and SON, univariate extended derivative ratio (EDR) method and multivariate partial least-squares (PLS) and principal component regression (PCR) methods were used for constructing the calibration curves. The extended derivative ratio (EDR) absorption maxima at 215 nm and minima at 310.5 nm was used for determination of RIV and DAV, respectively and absorption maxima at 240.3 nm and minima at 284.5 nm for determination of SOV and SON, respectively. The linearity was established over the range of 6-42 μg mL-1, 4-16 μg mL-1, 10-70 μg mL-1, and 3-9 μg mL-1 for RIV, DAV, SOV and SON with correlation coefficient (r2) of 0.9997, 0.9997, 0.9999 and 0.9997, respectively. This method was effectively applied to pure, pharmaceutical preparations and to spiked human urine and plasma. PLS and PCR models were established for the determination of the studied drugs in the range of 6-42, 4-16, 10-70 and 3-9 μg mL-1 for RIV, DAV, SOV, and SON, respectively. Furthermore, updating the PLS model (PLS model update) were allowed for the determination of these drugs in spiked human urine, plasma and drug-dissolution test of their tablets. The obtained results were compared to official and reported method showing that there were no significant differences. The results of applying PLS and PCR models for evaluation of RIV, DAV, SOV, and SON in human urine samples as real samples were also encouraging. It is expected that the suitable features of the proposed method make it helpful for biological and clinical applications.
Collapse
Affiliation(s)
| | - Wafaa S Hassan
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| | - Manal S ElMasry
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| | - Abdalla A Shalaby
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| |
Collapse
|
|
20
|
Oraby M, Khorshed A, Abdul-Rahman E, Ali R, Elsutohy MM. A clinical study for the evaluation of pharmacokinetic interaction between daclatasvir and fluoxetine. J Pharm Biomed Anal 2019; 171:104-110. [PMID: 30981192 DOI: 10.1016/j.jpba.2019.03.065] [Citation(s) in RCA: 5] [Impact Index Per Article: 0.8] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 12/26/2018] [Revised: 03/25/2019] [Accepted: 03/30/2019] [Indexed: 12/15/2022]
Abstract
A simple and sensitive chromatographic method has been developed for the quantitative analysis of an antiviral agent, daclatasvir (DCV), that commonly prescribed for the treatment of hepatitis C viral (HCV) infection. The method was applied to detect DCV in human plasma and real blood samples collected from patients diagnosed with HCV and treated with DCV. The analysis strategy was based on recording the native fluorescence of DCV in plasma, after pre-column treatment to precipitate the plasma proteins using a readily applicable protocol. Chromatographic conductions, factors influencing the fluorescence and stability studies were also investigated. Furthermore, the method was validated according to the International Conference on Harmonization (ICH) guidelines and could be used to detect DCV in plasma over a linear range of 1.0-4000 ng/mL, with an acceptable sensitivity as the limit of detection (LOD) was 0.025 ng/mL. In addition, the study was extended to evaluate the pharmacokinetic interaction between DCV and a co-prescribed antidepressant drug, fluoxetine (FLX) in real blood samples, collected from volunteering patients who were diagnosed with HCV and treated with DCV alone or combined with FLX. The results showed a significant influence of FLX on the pharmacokinetic profile of DCV. The findings observed in this study could be used by clinical pharmacists to adjust the DCV dose, when combined with FLX, during the HCV treatment.
Collapse
Affiliation(s)
- Mohamed Oraby
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Sohag University, Sohag 82524, Egypt.
| | - Ahmed Khorshed
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Sohag University, Sohag 82524, Egypt
| | - Eman Abdul-Rahman
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Sohag University, Sohag 82524, Egypt
| | - Ramadan Ali
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71526, Egypt
| | - Mohamed M Elsutohy
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71526, Egypt; Current address: Schulich School of Engineering, University of Calgary, Calgary, AB T2N 4V8, Canada.
| |
Collapse
|
|
21
|
Sultan MA, Abou El-Alamin MM, Wark AW, Azab MM. Stability-indicating micellar enhanced spectro-fluorometric determination of Daclatasvir in its tablet and spiked human plasma. SPECTROCHIMICA ACTA. PART A, MOLECULAR AND BIOMOLECULAR SPECTROSCOPY 2019; 211:52-58. [PMID: 30503988 DOI: 10.1016/j.saa.2018.11.023] [Citation(s) in RCA: 0] [Impact Index Per Article: 0] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Track Full Text] [Subscribe] [Scholar Register] [Received: 08/14/2018] [Revised: 11/11/2018] [Accepted: 11/12/2018] [Indexed: 06/09/2023]
Abstract
A fast, simple and sensitive micellar enhanced spectrofluorimetric method is performed for the determination of Daclatasvir dihydrochloride (DAC) in its pharmaceutical dosage form and in spiked human plasma. The fluorescence intensity (FI) was measured at 367 nm after excitation at 300 nm. In aqueous solution, the FI of DAC was greatly enhanced by >110% in the presence of sodium dodecyl sulphate (SDS). The detection method was linear over the range of 12.93 to 161.60 ng/mL, with a limit of detection of 1.75 ng/mL. The proposed method was successfully applied to the determination of DAC in its pharmaceutical dosage form and the mean % recovery of DAC in spiked human plasma was 95.42 ± 2.52. The developed methodology was also extended to stress studies of DAC after exposure to different forced degradation conditions including acidic, alkaline, photolytic, thermal and oxidative environments.
Collapse
Affiliation(s)
- Maha A Sultan
- Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, 11795 Cairo, Egypt
| | - Maha M Abou El-Alamin
- Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, 11795 Cairo, Egypt
| | - Alastair W Wark
- Centre for Molecular Nanometrology, WESTChem, Dept. of Pure & Applied Chemistry, Technology & Innovation Centre, University of Strathclyde, Glasgow G1 1RD, UK
| | - Marwa M Azab
- Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, 11795 Cairo, Egypt.
| |
Collapse
|
|
22
|
Abdel-Lateef MA, Omar MA, Ali R, Derayea SM. Xanthene based spectroscopic probe for the analysis of HCV antiviral, daclatasvir dihydrochloride, through feasible complexation reaction. Microchem J 2019. [DOI: 10.1016/j.microc.2018.11.038] [Citation(s) in RCA: 15] [Impact Index Per Article: 2.5] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 12/28/2022]
|
|
23
|
Ali R, Elsutohy MM. Specific, highly sensitive and simple spectrofluorimetric method for quantification of daclatasvir in HCV human plasma patients and in tablets dosage form. OPEN CHEM 2019. [DOI: 10.1515/chem-2019-0012] [Citation(s) in RCA: 2] [Impact Index Per Article: 0.3] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/15/2022] Open
Abstract
AbstractA simple, selective and highly sensitive spectrofluorimetric method for the quantitative detection of an antiviral drug, daclatasvir (DCV) has been developed and analytically validated in its pure form, in its commercially available pharmaceutical preparations, and in hepatitis-C (HCV) patient’s plasma. The method was based on recording the native fluorescence of DCV that exhibit an emission wavelength maximum at 380 nm upon excitation at 320 nm. Many factors affecting the fluorescence intensity and the method sensitivity including pH, type of surfactant and solvent have been studied and optimized. In addition, a stability-indicating study was performed in accordance with the guidelines of the International Conference on Harmonization (ICH), to detect the drug in the presence of its degradation products which validates the method for application in quality control laboratories. In addition, extraction of DCV from the plasma proteins was performed using a simple technique that was based on using methanol and borate buffer (pH 9) that gave a recovery of ~95%. The results showed that DCV could be detected using this method in the pure form (with a linear range of 2-1000 ng/mL), commercially available tablets and in plasma samples (with a linear range of 5-1000 ng/mL), without any interferences. Furthermore, the method was also analytically and clinically validated according to the Food and Drug Administration (FDA) guidelines, with limit of detection (LOD) of 0.3 and 0.5 ng/mL for DCV in the pure form and plasma samples, respectively.
Collapse
Affiliation(s)
- Ramadan Ali
- Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University, Assiut71524, Egypt
| | - Mohamed M Elsutohy
- Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University, Assiut71524, Egypt
| |
Collapse
|
|
24
|
Hendawy HAM, Eldin GMG, Fekry AM. A Zirconium Oxide Nanoparticle Modified Screen‐printed Electrode for Anodic Stripping Determination of Daclatasvir Dihydrochloride. ELECTROANAL 2019. [DOI: 10.1002/elan.201800841] [Citation(s) in RCA: 9] [Impact Index Per Article: 1.5] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 12/12/2022]
Affiliation(s)
- Hassan A. M. Hendawy
- National Organization for Drug Control and Research (NODCAR) P. O. Box 29 Cairo Egypt
| | - Ghada M. G. Eldin
- National Organization for Drug Control and Research (NODCAR) P. O. Box 29 Cairo Egypt
| | - Amany M. Fekry
- Chemistry DepartmentFaculty of Science, Cairo University Giza- 12613 Egypt
| |
Collapse
|
|
25
|
Jagadabi V, Nagendra Kumar PV, Mahesh K, Pamidi S, Ramaprasad LA, Nagaraju D. A Stability-Indicating UPLC Method for the Determination of Potential Impurities and Its Mass by a New QDa Mass Detector in Daclatasvir Drug Used to Treat Hepatitis C Infection. J Chromatogr Sci 2019; 57:44-53. [PMID: 30169761 DOI: 10.1093/chromsci/bmy079] [Citation(s) in RCA: 10] [Impact Index Per Article: 1.7] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 04/08/2016] [Indexed: 11/13/2022]
Abstract
A stability-indicating ultraperformance liquid chromatographic method has been developed for the quantitative determination of degradation products and process-related impurities of daclatasvir in a pharmaceutical dosage form. Chromatographic separation was achieved on a polar Waters ACQUITY BEH phenyl 100 × 2.1 mm, 1.7-μm column using the gradient program consisting of mobile phase A: 0.03 M sodium perchlorate with 0.002 M of 1-octanesulfonic acid sodium salt (pH 2.5 buffer) and mobile phase B: 0.03 M sodium perchlorate with 0.02 M of 1-octanesulfonic acid sodium salt (pH 2.5 buffer) with acetonitrile in the ratio of 20:80% v/v. A flow rate of 0.4 mL/min is maintained under ultraviolet detection at 305 nm. The run time was 15 min, within which daclatasvir, its related impurities and unknown degradants were well resolved. The method was found to produce symmetric and sharp peaks with good separation between process-related impurities and degradation impurities. Samples were subjected to hydrolysis (acid and base), oxidative, photolytic and thermal stress conditions to prove the stability-indicating nature of the method. The unknown degradation products were identified by PDA/QDa mass detector. This mass spectrum reveals protonated molecular ion peaks [M + H]+ at m/z DP1-582.4 in acid and base hydrolyses and m/z DP2-778.5 in peroxide hydrolysis. The method was validated in terms of specificity, precision, linearity, accuracy, limit of detection, limit of quantification and robustness as per ICH guidelines.
Collapse
Affiliation(s)
- Varaprasad Jagadabi
- Department of Chemistry, School of Technology, GITAM University, Hyderabad Campus, Hyderabad, Telangana, India.,Analytical R&D, Hetero Labs Ltd, Hyderabad, Telangana, India
| | - P V Nagendra Kumar
- Department of Chemistry, School of Technology, GITAM University, Hyderabad Campus, Hyderabad, Telangana, India
| | - Kasthuri Mahesh
- Department of Chemistry, School of Technology, GITAM University, Hyderabad Campus, Hyderabad, Telangana, India
| | | | - L A Ramaprasad
- Analytical R&D, Hetero Labs Ltd, Hyderabad, Telangana, India
| | - D Nagaraju
- Analytical R&D, Hetero Labs Ltd, Hyderabad, Telangana, India
| |
Collapse
|
|
26
|
Abdel-Lateef MA, Omar MA, Ali R, Derayea SM. Micellar spectrofluorimetric protocol for the innovative determination of HCV antiviral (daclatasvir) with enhanced sensitivity: Application to human plasma and stability study. SPECTROCHIMICA ACTA. PART A, MOLECULAR AND BIOMOLECULAR SPECTROSCOPY 2019; 206:57-64. [PMID: 30081268 DOI: 10.1016/j.saa.2018.07.101] [Citation(s) in RCA: 21] [Impact Index Per Article: 3.5] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Track Full Text] [Subscribe] [Scholar Register] [Received: 05/30/2018] [Revised: 07/17/2018] [Accepted: 07/31/2018] [Indexed: 06/08/2023]
Abstract
Daclatasvir dihydrochloride (DAC) is a new, direct-acting antiviral drug with powerful inhibitory effect against all hepatitis C virus (HCV) genotypes. A sensitive, simple, fast and specific fluorometric method for estimation of DAC in the presence of sofosbuvir was developed and validated. The method is based on reinforcement the fluorescence intensity of DAC by 170% of its original value in an aqueous solution of hexadecyl trimethyl ammonium bromide (pH 5.5, Teorell and Stenhagen buffer). The fluorescence intensity measurements were accomplished at 387 nm with 328 nm for excitation wavelength. A linear relationship was achieved between the DAC concentration and the fluorescence intensity in a range of 50.0-2000.0 ng ml-1 with 0.9998 and 0.9999 for the determination and correlation coefficients, respectively. The detection and quantitation limits were 13.4, 40.8 ng ml-1, respectively. The excellent sensitivity and specificity of the proposed method allowed the efficient estimation of DAC in real human plasma with adequate recovery (81.78 ± 1.57), and the selective determination for DAC in its commercial dosage form without interference from tablet excipient. Moreover, the proposed method was expanded to examine the stability of DAC by determination the parent drug of DAC in the presence of its oxidative, alkaline, acidic, UV, daylight and sunlight degradations products in agreement with ICH guidelines. Furthermore, the kinetic study of acidic and oxidative degradations of DAC was inspected. In addition, the half-life times of the reaction (t1/2) and the first-order reaction rate constants were estimated. Moreover, a suggestion for the degradation pathway was supposed.
Collapse
Affiliation(s)
- Mohamed A Abdel-Lateef
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71524, Egypt
| | - Mahmoud A Omar
- Department of Analytical Chemistry, Faculty of Pharmacy, Minia University, Minia 61519, Egypt.
| | - Ramadan Ali
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71524, Egypt
| | - Sayed M Derayea
- Department of Analytical Chemistry, Faculty of Pharmacy, Minia University, Minia 61519, Egypt
| |
Collapse
|
|
27
|
Salmon D, Trimoulet P, Gilbert C, Solas C, Lafourcade E, Chas J, Piroth L, Lacombe K, Katlama C, Peytavin G, Aumaitre H, Alric L, Boué F, Morlat P, Poizot-Martin I, Billaud E, Rosenthal E, Naqvi A, Miailhes P, Bani-Sadr F, Esterle L, Carrieri P, Dabis F, Sogni P, Wittkop L, ANRS CO13 Hepavih study Group. Factors associated with DAA virological treatment failure and resistance-associated substitutions description in HIV/HCV coinfected patients. World J Hepatol 2018; 10:856-866. [PMID: 30533186 PMCID: PMC6280155 DOI: 10.4254/wjh.v10.i11.856] [Citation(s) in RCA: 7] [Impact Index Per Article: 1.0] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Download PDF] [Journal Information] [Submit a Manuscript] [Subscribe] [Scholar Register] [Received: 06/14/2018] [Revised: 09/10/2018] [Accepted: 10/10/2018] [Indexed: 02/06/2023] Open
Abstract
AIM To describe factors associated with treatment failure and frequency of resistance-associated substitutions (RAS).
METHODS Human immunodeficiency virus (HIV)/hepatitis C virus (HCV) coinfected patients starting a first direct-acting antiviral (DAA) regimen before February 2016 and included in the French ANRS CO13 HEPAVIH cohort were eligible. Failure was defined as: (1) non-response [HCV-RNA remained detectable during treatment, at end of treatment (EOT)]; and (2) relapse (HCV-RNA suppressed at EOT but detectable thereafter). Sequencing analysis was performed to describe prevalence of drug class-specific RAS. Factors associated with failure were determined using logistic regression models.
RESULTS Among 559 patients, 77% had suppressed plasma HIV-RNA < 50 copies/mL at DAA treatment initiation, 41% were cirrhotic, and 68% were HCV treatment-experienced. Virological treatment failures occurred in 22 patients and were mainly relapses (17, 77%) then undefined failures (3, 14%) and non-responses (2, 9%). Mean treatment duration was 16 wk overall. Post-treatment NS3, NS5A or NS5B RAS were detected in 10/14 patients with samples available for sequencing analysis. After adjustment for age, sex, ribavirin use, HCV genotype and treatment duration, low platelet count was the only factor significantly associated with a higher risk of failure (OR: 6.5; 95%CI: 1.8-22.6).
CONCLUSION Only 3.9% HIV-HCV coinfected patients failed DAA regimens and RAS were found in 70% of those failing. Low platelet count was independently associated with virological failure.
Collapse
Affiliation(s)
- Dominique Salmon
- Assistance Publique des Hôpitaux de Paris, Hôpitaux Universitaires Paris Centre, Hôpital Hôtel Dieu, Unité des Maladies infectieuses et tropicales, Paris 75004, France
- Université Paris Descartes, Sorbonne Paris Cité, Paris 75006, France
| | - Pascale Trimoulet
- CHU de Bordeaux, Hôpital Pellegrin, Laboratoire de Virologie, Bordeaux 33000, France
- CNRS-UMR 5234, Microbiologie fondamentale et Pathogénicité, Université de Bordeaux, Bordeaux 3000, France
| | - Camille Gilbert
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
| | - Caroline Solas
- APHM, Hôpital La Timone, Laboratoire de Pharmacocinétique et Toxicologie, Marseille 13005, France
| | - Eva Lafourcade
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
| | - Julie Chas
- Assistance Publique des Hôpitaux de Paris, Hôpital Tenon, Service Maladies infectieuses et tropicales, Paris 75020, France
| | - Lionel Piroth
- Centre Hospitalier Universitaire de Dijon, Département d’Infectiologie, Dijon cedex 21079, France
- INSERM-CIC 1342 Université de Bourgogne, Dijon 21000, France
| | - Karine Lacombe
- Assistance Publique des Hôpitaux de Paris, GHUEP site Saint-Antoine, Services Maladies infectieuses et tropicales, Paris 75011, France
- Université Pierre et Marie Curie, UMR S1136, Institut Pierre Louis d’Epidémiologie et de Santé Publique, Paris 75646, France
| | - Christine Katlama
- Université Paris-Sorbonne, Paris 75005, France
- Assistance Publique des Hôpitaux de Paris Hôpital Pitié Salpêtrière, Services Maladies infectieuses et tropicales, Paris 75013, France
| | - Gilles Peytavin
- Assistance Publique des Hôpitaux de Paris, Hôpital Bichat-Claude Bernard, Laboratoire de Pharmacologie, Paris 75877, France
- IAME, UMR 1137, Sorbonne Paris Cité, INSERM, Université Paris Diderot, Paris 75890, France
| | - Hugues Aumaitre
- Centre Hospitalier de Perpignan, Service Maladies infectieuses et tropicales, Perpignan 66000, France
| | - Laurent Alric
- Centre Hospitalier Universitaire de Toulouse, Hôpital Purpan, Service Médecine interne-Pôle Digestif, Toulouse 31300, France
- UMR 152 IRD Université Toulouse III, Paul Sabatier, Toulouse 31330, France
| | - François Boué
- Hôpital Antoine-Béclère, Assistance Publique des Hôpitaux de Paris, Université Paris Sud, Service Médecine interne et immunologie, Clamart 92140, France
| | - Philippe Morlat
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
- Centre Hospitalier Universitaire de Bordeaux, Service de médecine interne, Hôpital Saint-André, Bordeaux 33000, France
| | - Isabelle Poizot-Martin
- Aix-Marseille Univ, APHM Sainte-Marguerite, Service d’Immuno-hématologie clinique, Marseille 13274, France
- Sciences Economiques and Sociales de la Santéand Traitement de l’Information Médicale, UMR912 INSERM, Aix-Marseille Université, IRD, Marseille 13009, France
| | - Eric Billaud
- Department of Infectious Diseases, CHU de Nantes and CIC 1413, Inserm, Nantes 44000, France
| | - Eric Rosenthal
- Centre Hospitalier Universitaire de Nice, Service de Médecine Interne, Hôpital l’Archet, Nice 06202, France
- Université de Nice-Sophia Antipolis, Nice 06100, France
| | - Alissa Naqvi
- Centre Hospitalier Universitaire de Nice, Service d’Infectiologie, Hôpital l’Archet, Nice 06100, France
| | - Patrick Miailhes
- Service des Maladies Infectieuses et Tropicales, Hospices Civils de Lyon, Hôpital de la Croix Rousse, Lyon 69004, France
| | - Firouzé Bani-Sadr
- Centre Hospitalier Universitaire de Reims, Service de Médecine Interne, Maladies Infectieuses et Immunologie Clinique, Reims 51100, France
- Faculté de Médecine EA-4684/SFR CAP-SANTE, Université de Reims, Champagne-Ardenne, Reims 51100, France
| | - Laure Esterle
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
| | - Patrizia Carrieri
- Sciences Economiques and Sociales de la Santéand Traitement de l’Information Médicale, UMR912 INSERM, Aix-Marseille Université, IRD, Marseille 13009, France
| | - François Dabis
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
| | - Philippe Sogni
- Assistance Publique des Hôpitaux de Paris, Hôpital Cochin, Service d’Hépatologie, Paris 75014, France
- Inserm U-1223 - Institut Pasteur, Paris 75015, France
| | - Linda Wittkop
- Univ. Bordeaux, ISPED, Inserm, Bordeaux Population Health Research Center, team MORPH3EUS, UMR 1219, CIC-EC 1401, Bordeaux F-33000, France
- CHU de Bordeaux, Pôle de santé Publique, Service dâinformation médicale, Bordeaux F-33000, France
| | | |
Collapse
|
|
28
|
Aboshabana R, Shalan S, Eid M, El-Enany N. Two validated spectrofluorimeteric and high performance liquid chromatography (HPLC) methods with fluorescence detection for the analysis of a new anti-hepatitis C drug, daclatasvir hydrochloride, in raw material or tablet form and in biological fluids. LUMINESCENCE 2018; 33:1333-1345. [DOI: 10.1002/bio.3551] [Citation(s) in RCA: 6] [Impact Index Per Article: 0.9] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 04/05/2018] [Revised: 08/07/2018] [Accepted: 08/23/2018] [Indexed: 11/09/2022]
Affiliation(s)
- Rasha Aboshabana
- Department of Analytical Chemistry, Faculty of Pharmacy; University of Mansoura; Mansoura Egypt
| | - Shereen Shalan
- Department of Analytical Chemistry, Faculty of Pharmacy; University of Mansoura; Mansoura Egypt
| | - Manal Eid
- Department of Analytical Chemistry, Faculty of Pharmacy; University of Mansoura; Mansoura Egypt
| | - Nahed El-Enany
- Department of Analytical Chemistry, Faculty of Pharmacy; University of Mansoura; Mansoura Egypt
| |
Collapse
|
|
29
|
Development of a Robust UPLC Method for Simultaneous Determination of a Novel Combination of Sofosbuvir and Daclatasvir in Human Plasma: Clinical Application to Therapeutic Drug Monitoring. Int J Anal Chem 2018; 2018:6535816. [PMID: 30420886 PMCID: PMC6215565 DOI: 10.1155/2018/6535816] [Citation(s) in RCA: 8] [Impact Index Per Article: 1.1] [Reference Citation Analysis] [Abstract] [Track Full Text] [Download PDF] [Figures] [Journal Information] [Subscribe] [Scholar Register] [Received: 05/28/2018] [Accepted: 10/02/2018] [Indexed: 12/29/2022] Open
Abstract
A rapid and selective UPLC-DAD method was developed and validated for simultaneous analysis of the novel two-drug combination Darvoni® for the treatment of HCV: Sofosbuvir (SF)/Daclatasvir (DC) in human plasma using Ledipasvir as internal standard (IS) where the extraction process was conducted using automated SPE. Although the analysis of the combination after concomitant oral intake of two tablets of SF and DC individually was reported in literature, yet simultaneous analysis of this new combination in human plasma after a single oral dose was not previously reported. The adopted chromatographic separation was achieved on Waters® Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 µm) as a stationary phase using isocratic elution using a mobile phase system of ammonium formate (pH 3.5; 5 mM) and acetonitrile (60:40 v/v) pumped at a flow rate of 0.2 mL.min−1. The UV detection was carried out at 261 nm for SF and 318 nm for DC and IS. SF was eluted at 1.123 min while DC was eluted at 3.179 min. The proposed chromatographic method was validated in accordance with guidelines of FDA for bioanalytical method validation. A linear range was achieved in the range of 25-6400 and 50-12800 ng.mL−1 for SF and DC, respectively. The proposed UPLC-DAD method was found to be accurate with % bias ranging between -10.0-7.2 for SF and -6.9-8.0 for DC. Also it was proved to be precise with % CV for intraday precision ranging between 3.8-9.6 for SF and 2.8-9.2 for DC whereas interday precision ranged between 5.1-9.3 for SF and 3.7-9.1 for DC. Moreover, % extraction recovery ranged between 90.0-107.2 for SF and 93.1-108.0 for DC using the suggested method. The adopted chromatographic method was successfully applied to the therapeutic drug monitoring of SF and DC in healthy volunteers after the oral intake of one Darvoni® tablet.
Collapse
|
|
30
|
Saraya RE, Elhenawee M, Saleh H. Development of a highly sensitive high-performance thin-layer chromatography method for the screening and simultaneous determination of sofosbuvir, daclatasvir, and ledipasvir in their pure forms and their different pharmaceutical formulations. J Sep Sci 2018; 41:3553-3560. [PMID: 30048040 DOI: 10.1002/jssc.201800567] [Citation(s) in RCA: 21] [Impact Index Per Article: 3.0] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 05/24/2018] [Revised: 10/07/2018] [Accepted: 07/18/2018] [Indexed: 01/19/2023]
Abstract
The combination of sofosbuvir and daclatasvir or sofosbuvir and ledipasvir is now widely used as an ideal treatment for hepatitis C virus infection. For this purpose, a simple, sensitive, accurate, economic, and precise high-performance thin-layer chromatography was developed and validated for the determination of sofosbuvir, daclatasvir, and ledipasvir in their pure form as well as their different pharmaceutical products. The method used Merck high-performance thin-layer chromatography aluminum plates precoated with silica gel 60 F254 as a stationary phase and mobile phase consisting of methylene chloride/methanol/ethyl acetate/ammonia (25%) (6:1:4:1, v/v/v/v). This system was found to give compact symmetric peaks of sofosbuvir, daclatasvir, and ledipasvir with retardation factors of 0.27 ± 0.01, 0.50 ± 0.007, and 0.68 ± 0.008, respectively. The densitometric scanner was set at 275 nm using a deuterium lamp. The calibration curves were linear over the range of 100-3000 ng/spot for sofosbuvir, and daclatasvir, and range of 50-3000 ng/spot for ledipasvir. The detection limits were 22.5, 31.90, and 15.80 for sofosbuvir, daclatasvir, and ledipasvir. The quantitation limits were 67.50, 95.60, and 47.50 for sofosbuvir, daclatasvir, and ledipasvir. The proposed method was validated according to International Conference on Harmonization (ICH) guidelines and the results were acceptable.
Collapse
Affiliation(s)
- Roshdy E Saraya
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Port Said University, Port Said, Egypt
| | - Magda Elhenawee
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt
| | - Hanaa Saleh
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt
| |
Collapse
|
|
31
|
Nano-magnetite/ionic liquid crystal modifiers of carbon nanotubes composite electrode for ultrasensitive determination of a new anti-hepatitis C drug in human serum. J Electroanal Chem (Lausanne) 2018. [DOI: 10.1016/j.jelechem.2018.06.016] [Citation(s) in RCA: 22] [Impact Index Per Article: 3.1] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 01/12/2023]
|
|
32
|
Abdallah OM, Abdel-Megied AM, Gouda AS. Pharmacokinetic evaluation of daclatasvir and ledipasvir in healthy volunteers using a validated highly sensitive spectrofluorimetric method. LUMINESCENCE 2018; 33:1094-1100. [DOI: 10.1002/bio.3514] [Citation(s) in RCA: 3] [Impact Index Per Article: 0.4] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 03/10/2018] [Revised: 05/03/2018] [Accepted: 05/13/2018] [Indexed: 01/26/2023]
Affiliation(s)
- Ola M. Abdallah
- Analytical Chemistry Department, Faculty of Pharmacy; Al-Azhar University (Girls); Cairo Egypt
- Pharmaceutical Chemistry Department, Faculty of Pharmacy; Badr University in Cairo (BUC); Badr City Cairo Egypt
| | - Ahmed M. Abdel-Megied
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy and Pharmaceutical Manufacturing; Kafrelsheikh University; Kafrelsheikh City Egypt
| | | |
Collapse
|
|
33
|
Dogra A, Bhatt S, Magotra A, Sharma A, Kotwal P, Gour A, Wazir P, Singh G, Nandi U. Intervention of curcumin on oral pharmacokinetics of daclatasvir in rat: A possible risk for long-term use. Phytother Res 2018; 32:1967-1974. [PMID: 29806225 DOI: 10.1002/ptr.6123] [Citation(s) in RCA: 16] [Impact Index Per Article: 2.3] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 12/27/2017] [Revised: 04/03/2018] [Accepted: 05/02/2018] [Indexed: 12/16/2022]
Abstract
Curcumin, a natural diarylheptanoid, is extensively used as a food additive or dietary supplement on the regular basis. It is known to have potential to encumber the drug transporters and hepatic drug metabolizing enzymes that lead to pharmacokinetic interactions with drug or food. Daclatasvir is a new orally acting drug for the treatment of chronic Hepatitis C Virus infections. This is a substrate of P-glycoprotein and CYP3A4 that are involved in the major pharmacokinetic interaction. Hence, the studies' aim is to assess for any possible pharmacokinetic interactions. Pharmacokinetic studies of daclatasvir in presence or absence of curcumin were carried out in Wistar rats following oral administration. Parallelly, the oral pharmacokinetics of daclatasvir was also determined in the presence of ketoconazole or quinidine. Studies revealed that plasma level of daclatasvir was not altered significantly during concomitant single dose administration of curcumin, whereas significantly decreased upon pretreatment for 7 days with curcumin at high dose level. Ketoconazole and quinidine markedly increase daclatasvir exposure following concomitant administration with daclatasvir. It can be concluded that dose adjustment is unlikely to be required for intermittent use of curcumin at low dose but cautious for chronic and concomitant use of curcumin at a high dose.
Collapse
Affiliation(s)
- Ashish Dogra
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Shipra Bhatt
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Asmita Magotra
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Anjna Sharma
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Pankul Kotwal
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Abhishek Gour
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Priya Wazir
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Gurdarshan Singh
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| | - Utpal Nandi
- PK-PD, Toxicology and Formulation Division, CSIR-Indian Institute of Integrative Medicine, Jammu, India.,Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Integrative Medicine, Jammu, India
| |
Collapse
|
|
34
|
Simultaneous quantitation of two direct acting hepatitis C antivirals (sofosbuvir and daclatasvir) by an HPLC-UV method designated for their pharmacokinetic study in rabbits. J Pharm Biomed Anal 2018; 158:88-93. [PMID: 29864695 DOI: 10.1016/j.jpba.2018.05.028] [Citation(s) in RCA: 15] [Impact Index Per Article: 2.1] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 02/12/2018] [Revised: 05/14/2018] [Accepted: 05/18/2018] [Indexed: 01/26/2023]
Abstract
Sofosbuvir (SOF) and daclatasvir (DCS) are novel, recently developed direct acting antiviral agents characterized by potent anti-hepatitis C virus action. A fast and efficient HPLC-UV method was developed, validated and applied for simultaneous determination of SOF and DCS in pharmaceutical formulations and biological fluids based on coupling liquid-liquid extraction with ultrasound and dual wavelength detection at λmax; 260 and 313 nm for SOF and DCS, respectively. This approach provided simple, sensitive, specific and cost-effective determination of the SOF-DCS mixture with good recoveries of the analytes from plasma. Analytes were separated within 7 min on C18 analytical column with acetonitrile-10 mM acetate buffer of pH 5.0 at a flow rate of 1.0 mL min-1. The linear ranges were 1-20 μg mL-1 for SOF and 0.6-6 μg mL-1 for DCS with correlation coefficients ≥0.9995. The detection limits in spiked rabbit plasma were 0.20 and 0.19 μg mL-1 for SOF and DCS, respectively. The method was validated according to ICH and US-FDA guidelines. Finally, the method was successfully applied for simultaneous pharmacokinetic studies of SOF and DCS in rabbits using rofecoxib as internal standard.
Collapse
|
|
35
|
Hassouna M, Mohamed M. UV-Spectrophotometric and Stability Indicating RP-HPLC Methods for the Determination of the Hepatitis C Virus Inhibitor Sofosbuvir in Tablet Dosage Form. ACTA ACUST UNITED AC 2018. [DOI: 10.1080/22297928.2017.1410441] [Citation(s) in RCA: 7] [Impact Index Per Article: 1.0] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 10/17/2022]
Affiliation(s)
- M.E.M. Hassouna
- Chemistry Department, Faculty of Science, Beni-Suef University, 62514, Egypt
| | - M.A. Mohamed
- HIKMA group, Pharmaceutical Company, Beni-Suef, Egypt
| |
Collapse
|
|
36
|
Efficient HPTLC-dual wavelength spectrodensitometric method for simultaneous determination of sofosbuvir and daclatasvir: Biological and pharmaceutical analysis. J Pharm Biomed Anal 2018; 156:358-365. [PMID: 29753282 DOI: 10.1016/j.jpba.2018.04.049] [Citation(s) in RCA: 19] [Impact Index Per Article: 2.7] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 02/15/2018] [Revised: 03/27/2018] [Accepted: 04/26/2018] [Indexed: 01/08/2023]
Abstract
Sofosbuvir (SOF) and daclatasvir (DCS) are newly discovered anti-hepatitis C drugs that have direct antiviral activity. A novel and simple high-performance thin-layer chromatography (HPTLC) method was designed for simultaneous determination of SOF and DCS in miscellaneous matrices. The method adopts coupling HPTLC with dual wavelength spectrodensitometry. Consequently, this enabled sensitive, specific and cost-effective determination of the SOF-DCS mixture. The developed HPTLC procedure is based on a simple liquid-liquid extraction, enrichment of the analytes and subsequent chromatographic separation with UV detection. Separations were performed on HPTLC silica gel 60 F254 aluminum plates with a mobile phase consisting of ethyl acetate-isopropanol (85:15, v/v). Dual wavelength scanning was carried out in the absorbance mode at 265 and 311 nm for SOF and DCS, respectively. The linear ranges were 40-640 and 20-320 ng band-1 for SOF and DCS, respectively with correlation coefficients of ≥0.9997. The detection limits were 11.3 and 6.5 ng band-1 for SOF and DCS, respectively indicating high sensitivity of the proposed method. Consequently, this permits in vitro and in vivo application of the proposed method in human plasma with good percentage recovery (94.1-103.5%). Validation parameters were assessed according to ICH guidelines and US-FDA guidelines. Furthermore, the application was extended to analysis of SOF and DCS in their pharmaceutical formulations.
Collapse
|
|
37
|
Zidan DW, Hassan WS, Elmasry MS, Shalaby AA. Investigation of anti-Hepatitis C virus, sofosbuvir and daclatasvir, in pure form, human plasma and human urine using micellar monolithic HPLC-UV method and application to pharmacokinetic study. J Chromatogr B Analyt Technol Biomed Life Sci 2018; 1086:73-81. [PMID: 29660665 DOI: 10.1016/j.jchromb.2018.04.011] [Citation(s) in RCA: 11] [Impact Index Per Article: 1.6] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 01/30/2018] [Revised: 03/29/2018] [Accepted: 04/06/2018] [Indexed: 12/17/2022]
Abstract
Simultaneous determination of sofosbuvir (SOF), and daclatasvir (DAC) in their dosage forms, human urine and human plasma using simple and rapid micellar high performance liquid chromatographic method coupled with UV detection (HPLC-UV) had been developed and validated. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of Hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. Separation and quantitation were carried out on anonyx™ C8 monolithic (100 × 4.6 mm (i.d.) analytical column maintained at 25 °C. The mobile phase consisted of 0.1 M sodium dodecyl sulfate (SDS) solution containing 20% (V/V) n-propanolol and 0.3% (V/V) triethylamine and pH was adjusted to 6.5 using 0.02 M phosphoric acid, respectively. The retention times of SOF and DAC were 4.8 min, and 6.5 min, respectively. Measurements were made at flow rate of 0.5 mL/min with injection volume of 20 μL and ultraviolet (UV) detection at 226 nm. Linearity of SOF and DAC was obtained over concentration ranges of 50-400, and 40-400 ng/mL, respectively in pure form, 60-300 and 50-300 ng/mL, respectively for human plasma and over 50-400, and 40-400 ng/mL, respectively for human urine with correlation coefficient >0.999. The proposed method demonstrated excellent intra- and inter-day precision and accuracy. The suggested method was applied for determination of the drugs in pure, dosage form, and in real human plasma, real human urine and drug-dissolution test of their tablets. The obtained results have been statistically compared to reported method to give a conclusion that there is no significant differences.
Collapse
Affiliation(s)
| | - Wafaa S Hassan
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| | - Manal S Elmasry
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| | - Abdalla A Shalaby
- Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Egypt
| |
Collapse
|
|
38
|
Zaman B, Hassan W. Development of Stability Indicating HPLC–UV Method for Determination of Daclatasvir and Characterization of Forced Degradation Products. Chromatographia 2018. [DOI: 10.1007/s10337-018-3503-7] [Citation(s) in RCA: 17] [Impact Index Per Article: 2.4] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/29/2022]
|
|
39
|
Ibrahim AE, Hashem H, Elhenawee M, Saleh H. Comparison between core-shell and totally porous particle stationary phases for fast and green LC determination of five hepatitis-C antiviral drugs. J Sep Sci 2018; 41:1734-1742. [PMID: 29297968 DOI: 10.1002/jssc.201701263] [Citation(s) in RCA: 14] [Impact Index Per Article: 2.0] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 10/26/2017] [Revised: 12/19/2017] [Accepted: 12/20/2017] [Indexed: 12/12/2022]
Abstract
The performances of core-shell 2.7 μm and fully porous sub-2 μm particles packed in narrow diameter columns were compared under the same chromatographic conditions. The stationary phases were compared for fast separation and determination of five new antiviral drugs; daclatasvir, sofosbuvir, velpatasvir, simeprevir, and ledipasvir. The gradient elution was done using ethanol as green organic modifier, which is more environmentally friendly. Although both columns provided very good resolution of the five drugs, core-shell particles had proven to be of better efficiency. Under gradient elution conditions, core-shell particles exhibited faster elution, better peak shape, and enhanced resolution adding to lower system backpressure. The column backpressure on sub-2 μm particles was more than twice that on core-shell particles. This gives a chance to use conventional high-performance liquid chromatography conditions without needing special instrumentation as that required for ultra-high performance liquid chromatography. The method was validated for determination of the five drugs by gradient elution using mobile phase composed of organic modifier ethanol and aqueous part containing 0.75 g sodium octane sufonate and 3.0 g sodium dihydrogen phosphate per liter at pH of 6.15. Detection was done using UV-detector set at 210 nm. The linearity, accuracy, and precision were found very good within the concentration range of 2-200 μg/mL.
Collapse
Affiliation(s)
- Adel Ehab Ibrahim
- Egyptian International Pharmaceutical Industries Co. "EIPICo.", 10th of Ramadan City, Egypt
| | - Hisham Hashem
- Pharmaceutical analytical chemistry department, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt.,Chemistry department, Faculty of Science, Jazan University, Jizan, Saudi Arabia
| | - Magda Elhenawee
- Pharmaceutical analytical chemistry department, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt
| | - Hanaa Saleh
- Pharmaceutical analytical chemistry department, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt
| |
Collapse
|
|
40
|
Abo-Zeid MN, Atia NN, El-Gizawy SM, El-Shaboury SR. Ultrasensitive spectrofluorimetric method for rapid determination of daclatasvir and ledipasvir in human plasma and pharmaceutical formulations. J Pharm Biomed Anal 2018; 152:155-164. [PMID: 29414007 DOI: 10.1016/j.jpba.2018.01.038] [Citation(s) in RCA: 28] [Impact Index Per Article: 4.0] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 10/22/2017] [Revised: 01/16/2018] [Accepted: 01/18/2018] [Indexed: 01/29/2023]
Abstract
Direct-acting antivirals (DAAs) represent a revolution in the treatment of chronic hepatitis C which have emerged at an extremely rapid pace over the past few years. DAAs act directly on the hepatitis C virus at various points in the viral life cycle to inhibit viral production. Among these novel DAAs, are daclatasvir (DCS) and ledipasvir (LDS). Herein, a novel, fast, simple, ultrasensitive and cost-effective spectrofluorimetric method was designed for determination of DCS and LDS in miscellaneous matrices. The method is based on investigation of the native fluorescence of the cited drugs. The relative fluorescence intensity (RFI) was measured at λex/λem equal to 315/381 nm for DCS and 332/387 nm for LDS. Under the optimum conditions, the linear ranges of calibration curves were 0.2-30 and 6-120 ng mL-1 for DCS and LDS, respectively with correlation coefficients ≥0.9998. The detection limits were 0.047 and 1.939 ng mL-1 for DCS and LDS, respectively indicating ultrasensitivity of the proposed method. Consequently, this permits in vitro and in vivo application of the proposed method in spiked and real human plasma with good percentage recovery (96.6-103.6%). The method was validated in compliance with ICH guidelines and US-FDA guidelines. Furthermore, the application was extended to analysis of DCS and LDS in its pharmaceutical formulations (either alone or in presence of other co-formulated drugs) and in synthetic mixture with sofosbuvir or ribavirin.
Collapse
Affiliation(s)
- Mohammad Nabil Abo-Zeid
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt.
| | - Noha N Atia
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt
| | - Samia M El-Gizawy
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt
| | - Salwa R El-Shaboury
- Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71526, Egypt
| |
Collapse
|
|
41
|
Abdallah OM, Abdel-Megied AM, Gouda AS. Development and validation of LC-MS/MS method for simultaneous determination of sofosbuvir and daclatasvir in human Plasma: Application to pharmacokinetic study. Biomed Chromatogr 2018; 32:e4186. [PMID: 29314090 DOI: 10.1002/bmc.4186] [Citation(s) in RCA: 28] [Impact Index Per Article: 4.0] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 09/22/2017] [Revised: 12/13/2017] [Accepted: 12/20/2017] [Indexed: 01/17/2023]
Abstract
A simple and highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalytical method was developed and fully validated for the first time for the simultaneous determination of newly discovered antiviral drugs, namely sofosbuvir (SOF) and daclatasvir (DAC) in human plasma. Tadalafil (TAD) was used as internal standard (IS). SOF, DAC and TAD (IS) were extracted from plasma using liquid-liquid extraction technique with methyl tert-butyl ether. The chromatographic separation was carried out using ZorbaxSB-C18 column (4.6 × 50 mm,5 μm) and 5 mm ammonium formate buffer (pH 3.5)-acetonitrile (50:50, v/v) as mobile phase in an isocratic elution mode pumped at a flow rate 0.7 mL min-1 . The quantitation was performed on API4500 triple quadrupole tandem mass spectrometer with positive electrospray ionization interface in multiple reaction monitoring mode. Validation was applied according to US Food and Drug Administration guidelines for bio-analytical methodswith respect to linearity, precision, accuracy, selectivity, carry-over, stability and dilution integrity. Linearity was obtained over concentration ranges of 0.3-3000 and 3-3000 ng mL-1 for SOF and DAC, respectively, by applying a weighted least-squares linear regression method (1/x2 ). The proposed method could be applied successfully in bioequivalence and/or clinical studies for therapeutic drug monitoring of patients undergoing dual combination therapy as the latter combination proved more efficacious and powerful tool for the complete treatment of hepatitis C genotype 3 within 16 weeks. The suggested method has been applied successfully to pharmacokinetic studies with excellent assay ruggedness and reproducibility.
Collapse
Affiliation(s)
- Ola M Abdallah
- Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University (Girls), Cairo, Egypt.,Pharmaceutical Chemistry Department, Faculty of Pharmacy, Badr University in Cairo (BUC), Badr City, Cairo, Egypt
| | - Ahmed M Abdel-Megied
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy and Pharmaceutical Manufacturing, Kafrelsheikh University, Kafrelsheikh City, Egypt
| | | |
Collapse
|
|
42
|
Notari S, Tempestilli M, Fabbri G, Libertone R, Antinori A, Ammassari A, Agrati C. UPLC-MS/MS method for the simultaneous quantification of sofosbuvir, sofosbuvir metabolite (GS-331007) and daclatasvir in plasma of HIV/HCV co-infected patients. J Chromatogr B Analyt Technol Biomed Life Sci 2017; 1073:183-190. [PMID: 29276983 DOI: 10.1016/j.jchromb.2017.12.018] [Citation(s) in RCA: 25] [Impact Index Per Article: 3.1] [Reference Citation Analysis] [Abstract] [Key Words] [Journal Information] [Subscribe] [Scholar Register] [Received: 07/04/2017] [Revised: 12/06/2017] [Accepted: 12/10/2017] [Indexed: 01/21/2023]
Abstract
Direct-acting antiviral agents (DAAs) represent the major advance in hepatitis C virus (HCV) infection treatment leading to extremely high eradication rates in HCV mono- and HIV/HCV co-infected patients. In this scenery, availability of Therapeutic Drug Monitoring (TDM) is of interest to assess plasma concentrations to prevent either therapeutic failure due to suboptimal medication adherence and drug-drug interactions or avoid adverse events. Aim of this study was to develop and validate an Ultra-Performance Liquid Chromatography Mass Spectrometry (UPLC-MS/MS) method for the simultaneous quantification of sofosbuvir, sofosbuvir metabolite (GS-331007), and daclatasvir in human plasma. A simple protein precipitation was applied by adding 200 μL acetonitrile with internal standard 6,7-Dimethyl- 2,3-di(2-pyridyl) quinoxaline to 100 μL plasma sample. Drug separation was performed on analytical C-18 Luna Omega column (50 mm × 2.1 mm I.D.) with particle size of 1.6 μm. The mobile phase consisting of water containing 0.1% formic acid and acetonitrile at flow 0.4 mL/min and a gradient run time of 3.5 min. The injection volume was 10 μL. Anti-HCV drugs were detected in positive electrospray ionization mode. The full scan mass spectral analyses of sofosbuvir, GS-331007, daclatasvir and quinaxoline showed protonated molecule ions and transitions m/z: 530.098 → 243.02, 260.93 → 112.94, 739.4 → 339.27 and 313.03 → 77.99 respectively. The linearity of standard curves was excellent (r2 > 0.99), the absolute recovery of anti-HCV drugs ranged between 95 and 98%, and both imprecision and inaccuracy were <15% according to FDA guidelines. The UPLC-MS/MS method was applied to 16 plasma samples of as many HIV/HCV co-infected patients treated with sofosbuvir and daclatasvir. While sofosbuvir was not detectable in all samples, the median plasma concentrations of daclatasvir and GS-331007 were 223.6 ± 319.56 ng/mL and 537.11 ± 242.09 ng/mL, respectively. In conclusion, we describe an UPLC-MS/MS method allowing the simultaneous quantification of sofosbuvir, GS-331007 and daclatasvir in plasma samples. The method was sensitive, specific, robust, and time-saving.
Collapse
Affiliation(s)
- Stefania Notari
- Laboratory of Cellular Immunology and Pharmacology, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Massimo Tempestilli
- Laboratory of Cellular Immunology and Pharmacology, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Gabriele Fabbri
- Clinical Department, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Raffaella Libertone
- Clinical Department, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Andrea Antinori
- Clinical Department, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Adriana Ammassari
- Clinical Department, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy
| | - Chiara Agrati
- Laboratory of Cellular Immunology and Pharmacology, National Institute for Infectious Diseases "Lazzaro Spallanzani", IRCCS, Rome, Italy.
| |
Collapse
|
|
43
|
Nováková L, Pavlík J, Chrenková L, Martinec O, Červený L. Current antiviral drugs and their analysis in biological materials - Part II: Antivirals against hepatitis and HIV viruses. J Pharm Biomed Anal 2017; 147:378-399. [PMID: 29031512 DOI: 10.1016/j.jpba.2017.07.003] [Citation(s) in RCA: 31] [Impact Index Per Article: 3.9] [Reference Citation Analysis] [Abstract] [Key Words] [MESH Headings] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 06/30/2017] [Accepted: 07/01/2017] [Indexed: 12/18/2022]
Abstract
This review is a Part II of the series aiming to provide comprehensive overview of currently used antiviral drugs and to show modern approaches to their analysis. While in the Part I antivirals against herpes viruses and antivirals against respiratory viruses were addressed, this part concerns antivirals against hepatitis viruses (B and C) and human immunodeficiency virus (HIV). Many novel antivirals against hepatitis C virus (HCV) and HIV have been introduced into the clinical practice over the last decade. The recent broadening portfolio of these groups of antivirals is reflected in increasing number of developed analytical methods required to meet the needs of clinical terrain. Part II summarizes the mechanisms of action of antivirals against hepatitis B virus (HBV), HCV, and HIV, their use in clinical practice, and analytical methods for individual classes. It also provides expert opinion on state of art in the field of bioanalysis of these drugs. Analytical methods reflect novelty of these chemical structures and use by far the most current approaches, such as simple and high-throughput sample preparation and fast separation, often by means of UHPLC-MS/MS. Proper method validation based on requirements of bioanalytical guidelines is an inherent part of the developed methods.
Collapse
Affiliation(s)
- Lucie Nováková
- Department of Analytical Chemistry, Faculty of Pharmacy in Hradec Králové, Charles University, Akademika Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
| | - Jakub Pavlík
- Department of Analytical Chemistry, Faculty of Pharmacy in Hradec Králové, Charles University, Akademika Heyrovského 1203, 500 05 Hradec Králové, Czech Republic
| | - Lucia Chrenková
- Department of Analytical Chemistry, Faculty of Pharmacy in Hradec Králové, Charles University, Akademika Heyrovského 1203, 500 05 Hradec Králové, Czech Republic
| | - Ondřej Martinec
- Department of Pharmacology and Toxicology, Faculty of Pharmacy in Hradec Králové, Charles University, Akademika Heyrovského 1203, 500 05 Hradec Králové, Czech Republic
| | - Lukáš Červený
- Department of Pharmacology and Toxicology, Faculty of Pharmacy in Hradec Králové, Charles University, Akademika Heyrovského 1203, 500 05 Hradec Králové, Czech Republic
| |
Collapse
|
|
44
|
Reversed-Phase Liquid Chromatographic Method for Determination of Daclatasvir Dihydrochloride and Study of Its Degradation Behavior. Chromatographia 2017. [DOI: 10.1007/s10337-017-3321-3] [Citation(s) in RCA: 11] [Impact Index Per Article: 1.4] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 10/19/2022]
|
|
45
|
Baker MM, El-Kafrawy DS, Mahrous MS, Belal TS. Validated stability-indicating HPLC-DAD method for determination of the recently approved hepatitis C antiviral agent daclatasvir. ANNALES PHARMACEUTIQUES FRANÇAISES 2017; 75:176-184. [PMID: 28187879 DOI: 10.1016/j.pharma.2016.12.005] [Citation(s) in RCA: 20] [Impact Index Per Article: 2.5] [Reference Citation Analysis] [Abstract] [Key Words] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 10/27/2016] [Revised: 12/12/2016] [Accepted: 12/16/2016] [Indexed: 11/26/2022]
Abstract
A comprehensive stability indicating HPLC with diode array detection method was developed for the determination of the recently approved antiviral drug daclatasvir dihydrochloride (DCV) which is used for the treatment of chronic Hepatitis C Virus (HCV) genotype 3 infection. Effective chromatographic separation was achieved using Waters C8 column (4.6×250mm, 5μm particle size) with isocratic elution of the mobile phase composed of mixed phosphate buffer pH 2.5 and acetonitrile in the ratio of 75:25 (by volume). The mobile phase was pumped at a flow rate of 1.2mL/min, and quantification of DCV was based on measuring its peak areas at 306nm. DCV eluted at retention time 5.4min. Analytical performance of the proposed HPLC procedure was thoroughly validated with respect to system suitability, linearity, range, precision, accuracy, specificity, robustness, detection and quantification limits. The linearity range was 0.6-60μg/mL with correlation coefficient>0.99999. The drug was subjected to forced degradation conditions of neutral, acidic and alkaline hydrolysis, oxidation and thermal degradation. The proposed method proved to be stability-indicating by resolution of the drug from its forced-degradation products. The validated HPLC method was successfully applied to analysis of the cited drug in its tablets.
Collapse
Affiliation(s)
- M M Baker
- Methodology Department, Pharco Pharmaceuticals Company, Alexandria, Egypt
| | - D S El-Kafrawy
- Pharmaceutical Chemistry Department, Faculty of Pharmacy, University of Alexandria, Elmessalah, 21521 Alexandria, Egypt
| | - M S Mahrous
- Pharmaceutical Chemistry Department, Faculty of Pharmacy, University of Alexandria, Elmessalah, 21521 Alexandria, Egypt
| | - T S Belal
- Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, University of Alexandria, Elmessalah, 21521 Alexandria, Egypt.
| |
Collapse
|
|
46
|
Nannetti G, Messa L, Celegato M, Pagni S, Basso M, Parisi SG, Palù G, Loregian A. Development and validation of a simple and robust HPLC method with UV detection for quantification of the hepatitis C virus inhibitor daclatasvir in human plasma. J Pharm Biomed Anal 2017; 134:275-281. [DOI: 10.1016/j.jpba.2016.11.032] [Citation(s) in RCA: 31] [Impact Index Per Article: 3.9] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Received: 09/07/2016] [Revised: 11/07/2016] [Accepted: 11/13/2016] [Indexed: 11/16/2022]
|
|
47
|
Azab S, Fekry AM. Electrochemical design of a new nanosensor based on cobalt nanoparticles, chitosan and MWCNT for the determination of daclatasvir: a hepatitis C antiviral drug. RSC Adv 2017. [DOI: 10.1039/c6ra25826c] [Citation(s) in RCA: 63] [Impact Index Per Article: 7.9] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/21/2022] Open
Abstract
Daclatasvir (DAC) is listed on the World Health Organization's list of essential medicines needed in a basic health system, therefore, electrochemical and impedance spectroscopic methods are necessary.
Collapse
Affiliation(s)
- Shereen M. Azab
- Pharmaceutical Chemistry Dept
- National Organization for Drug Control and Research [NODCAR]
- Giza
- Egypt
| | - Amany M. Fekry
- Chemistry Department
- Faculty of Science
- Cairo University
- Giza-12613
- Egypt
| |
Collapse
|
|
48
|
Azab SM, Fekry AM. The application of a bee glue-modified sensor in daclatasvir dual effect detection. NEW J CHEM 2017. [DOI: 10.1039/c7nj01517h] [Citation(s) in RCA: 17] [Impact Index Per Article: 2.1] [Reference Citation Analysis] [Abstract] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 11/21/2022]
Abstract
A simple and novel carbon paste sensor containing chemically mixed propolis (bee glue) and graphene oxide (GO) was prepared, then electrochemical deposition of silver nanoparticles (AgNPs) was performed to fabricate a selective and sensible electrochemical sensor to detect Daclatasvir (DAC).
Collapse
Affiliation(s)
- Shereen M. Azab
- Pharmaceutical Chemistry Dept., National Organization for Drug Control and Research
- Giza
- Egypt
| | - Amany M. Fekry
- Chemistry Department, Faculty of Science, Cairo University
- Giza
- Egypt
| |
Collapse
|
|
49
|
Development and Validation of the Chiral HPLC Method for Daclatasvir in Gradient Elution Mode on Amylose-Based Immobilized Chiral Stationary Phase. Chromatographia 2016. [DOI: 10.1007/s10337-016-3157-2] [Citation(s) in RCA: 14] [Impact Index Per Article: 1.6] [Reference Citation Analysis] [Track Full Text] [Journal Information] [Subscribe] [Scholar Register] [Indexed: 01/30/2023]
|