Chemometrically Assisted Development of Ultra-High-Performance Liquid Chromatography Method for the Simultaneous Quantification of Sofosbuvir, Daclatasvir and Ledipasvir in Pharmaceutical Dosage Forms

2019 ◽  
Vol 57 (10) ◽  
pp. 910-919
Author(s):  
Aymen Labidi ◽  
Latifa Latrous El Atrache
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Fractional Factorial ◽  
Control Analysis ◽  
Dissolution Profile ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Simultaneous Quantification ◽  
Liquid Chromatography Method

Abstract A new ultra-high-performance liquid chromatography method for the simultaneous quantification of sofosbuvir, daclatasvir and ledipasvir was developed. Two combinations of these direct-acting antivirals are used in hepatitis C virus infection therapy and show high efficacy and safety. Fractional factorial design was used for screening the most influential factors on separation and time analysis. These significant factors were optimized using a central composite design. The optimum resolution was carried out by using a Waters XBridge C18 column (150 mm, 4.6 mm ID, 5 μm) at a temperature of 35°C ± 2°C and acetonitrile/sodium perchlorate buffer (10 mM, pH = 3.2) (40: 60 v/v) as mobile phase at a flow rate of 1.5 mL min−1. UV detection was set at λ = 210 nm. A short chromatographic separation time was achieved. The developed method was validated according to the accuracy profile approach and was found specific, precise, faithful and accurate. The detection limits were between 0.07 and 0.13 μg mL−1. Hence, this novel method can be employed for the routine quality control analysis and in dissolution profile studies of generics containing these products.

DEVELOPMENT AND VALIDATION OF THE REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE ESTIMATION OF GUAIFENESIN IN METHOCARBAMOL API AND ITS PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (5) ◽  
pp. 401
Author(s):  
Mannem Durga Babu ◽  
Kesana Surendrababu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Solution Stability ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatography Method

Objective: The objective of the study was to develop and validate a novel, specific, precise, and simple reversed-phase high-performance liquid chromatography method for the estimation of guaifenesin present in methocarbamol API and its pharmaceutical dosage forms. Methods: The baseline separation for methocarbamol and guaifenesin was achieved by utilizing a Inertsil ODS C18 (250 mm × 4.6 mm) 5 μm column particle size and an isocratic elution method. The mobile phase contains a mixture of water and acetonitrile in the ratio of 70:30 v/v, respectively. The flow rate of the mobile phase was 1.0 mL/min with a column temperature of 25°C and detection wavelength at 272 nm. The method was validated for a limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and reproducibility with the help of the exhibit and simulated samples. Results: The LOD for guaifenesin was 0.62 μg/mL. The LOQ for guaifenesin was 1.87 μg/mL. The correlation coefficient obtained for impurity was >0.99. The recovery was obtained for impurity was 106.56% at 50%, 95.20% at 100%, and 100.45% at 150%. In tablet analysis, we can found 0.26% (<0.5%). Conclusion: The developed method was validated as per the ICH guidelines with respect to specificity, precision, linearity, accuracy, LOD and quantification, ruggedness, robustness, and solution stability.

scholarly journals EVALUATION OF INNOVATED FORMULA OF BISACODYL SUPPOSITORY FOLLOWING THE DISSOLUTION PROFILE AND STABILITY DATA USING DEVELOPED HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2020 ◽  
Author(s):  
KAHTAN J HASSON ◽  
ESRAA G JABAR ◽  
IHAB I ALKHALIFA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Alkaline Medium ◽  
High Performance ◽  
Inclusion Complexation ◽  
Stability Study ◽  
Dissolution Profile ◽  
Chromatography Method ◽  
Beta Cyclodextrin ◽  
Liquid Chromatography Method

Objective: Bisacodyl is a laxative drug used in the treatment of constipation, it is soluble in mineral acids, but it is practically insoluble in water. Therefore, it is very hard task to dissolve bisacodyl in alkaline medium so the objective of this study was the development of proper dissolution method for a new formulation of bisacodyl suppositories in a medium simulated to rectal region. Obviously, most of the bisacodyl suppositories preparation products will yield low percentages of dissolution in the alkaline medium of phosphate buffer pH 7.2. Methods: Preparation inclusion complex of bisacodyl with the solubilizing agent beta-cyclodextrin then incorporated in a suppository base. The quantitative analysis of bisacodyl in suppositories was carried by a developed and validated high-performance liquid chromatography method. Results and Discussion: The dissolution rates for the innovated formulation of bisacodyl complexed with beta-cyclodextrin suppositories were in average of 97.5% and the stored suppositories of this formulation maintained their specified physical and chemical properties along the real stability study. Conclusion: The application of the inclusion complexation technique of bisacodyl with beta-cyclodextrin in the production of suppositories enhances the dissolution rate and improves the stability of suppositories performance.

scholarly journals Validation of analytical methodology for quantification of cefazolin sodium pharmaceutical dosage form by high performance liquid chromatography to be applied for quality control in pharmaceutical industry

2014 ◽  
Vol 50 (1) ◽  
pp. 213-223 ◽  
Author(s):  
Tahisa Marcela Pedroso ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Pharmaceutical Industry ◽  
High Performance ◽  
Fractional Factorial ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Cefazolin Sodium ◽  
Liquid Chromatography Method

A reversed-phase high performance liquid chromatography method was validated for the determination of cefazolin sodium in lyophilized powder for solution for injection to be applied for quality control in pharmaceutical industry. The liquid chromatography method was conducted on a Zorbax Eclipse Plus C18 column (250 x 4.6 mm, 5 μm), maintained at room temperature. The mobile phase consisted of purified water: acetonitrile (60: 40 v/v), adjusted to pH 8 with triethylamine. The flow rate was of 0.5 mL min-1 and effluents were monitored at 270 nm. The retention time for cefazolin sodium was 3.6 min. The method proved to be linear (r2=0.9999) over the concentration range of 30-80 µg mL-1. The selectivity of the method was proven through degradation studies. The method demonstrated satisfactory results for precision, accuracy, limits of detection and quantitation. The robustness of this method was evaluated using the Plackett–Burman fractional factorial experimental design with a matrix of 15 experiments and the statistical treatment proposed by Youden and Steiner. Finally, the proposed method could be also an advantageous option for the analysis of cefazolin sodium, contributing to improve the quality control and to assure the therapeutic efficacy.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF EMTRICITABINE AND TENOFOVIR BY REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY IN BULK AND TABLET DOSAGE FORMS

2017 ◽  
Vol 10 (11) ◽  
pp. 59
Author(s):  
Sufiyan Ahmad ◽  
Mohammed Rageeb Mohammed Usman
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Tablet Dosage

  Objective: A simple rapid, accurate, precise, and reproducible validated reversed-phase high performance liquid chromatography method was developed for the determination of emtricitabine (EMB) and tenofovir (TEN) in bulk and tablet dosage forms.Methods: The quantification was carried out using symmetry Premsil C18 (250 mm×4.6 mm, 5 μm) Younglin (S.K.) gradient way using mobile phase comprising of methanol:water (70:30 v/v) pH 3 and a detection wavelength of 273 nm, and injection volume of 20 μL, with a flow rate of 1 ml/minutes.Results: In the developed method, the retention time of EMB and TEN were found to be 3.1667 minutes and 7.5000 minutes. The developed method was validated according to the International Conference on Harmonization (ICH) guidelines.Conclusion: The linearity, precision, range, robustness was within the limits as specified by the ICH guidelines. Hence, the method was found to be simple, accurate, precise, economic, and reproducible. Hence, it is worthwhile that the proposed methods can be successfully utilized for the routine quality control analysis EMB and TEN in bulk drug as well as in formulations.

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