scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING REVERSE-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF POTENTIAL DEGRADATION PRODUCTS OF REGADENOSON FROM ITS PARENTERAL DOSAGE FORM

2018 ◽  
Vol 11 (8) ◽  
pp. 277
Author(s):  
Murlidhar V Zope ◽  
Rahul M Patel ◽  
Ashwinikumari Patel ◽  
Samir G Patel
Keyword(s):  
Liquid Chromatography ◽  
Degradation Product ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method ◽  
Injectable Dosage

Objective: The objective was to develop and validate the stability indicating reverse-phase high-performance liquid chromatography method for the quantification of potential degradation products of regadenoson (REGA) from its injectable dosage form.Methods: YMC-PAK ODS AQ, 150 mm × 4.6 mm, 3 μm composed with hydrophobic high carbon loading and a relatively hydrophilic surface chemically bonded to porous silica particles column was used with the temperature maintained at 40°C. Mobile phase A composed of 0.1% triethylamine buffer having pH 4.5 while mobile phase B is 100 % acetonitrile was used for gradient elution with 1.5 ml/min as a flow rate. The wavelength used for quantification was 245 nm and 20 μl as an injection volume. The suitability of the method has been checked and validated according to the International Council for Harmonization (ICH) guidelines for different parameters, namely, specificity, linearity, accuracy, precision, limit of quantification (LOQ), Limit of detection (LOQ), and robustness studies.Results: The resolution between REGA and its two-degradation product is >8.0 for all pairs of components. The high correlation coefficient (r2>0.990) values are for drug and all potential degradation products from LOQ to 150% of specification limits for impurities calculated based on the maximum daily dose of REGA. LOQ for the drug as well as each degradation product is <0.02% w/w. The % relative standard deviation (RSD) for precision and intermediate precision is in the range of 0.17–0.89, and % RSD for precision at LOQ is 0.86–2.35. The % RSD for robustness study is maximum 2.59.Conclusion: The developed method can quantify the specified and unknown degradation products from 0.1% in the injectable dosage form which indicates that method is sensitive. Method fulfills the ICH criteria for its different validation parameters and demonstrates that the developed analytical method is highly specific, precise, and robust and would have a great value when applied in quality control and stability studies for REGA injection.

scholarly journals STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF APIGENIN AND LUTEOLIN FROM ACHILLEA MILLEFOLIUM LINN

2019 ◽  
pp. 169-172
Author(s):  
GOMATHY SUBRAMANIAN ◽  
S.N.MEYYANATHAN ◽  
GOWRAMMA BYRAN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Objective: A stability-indicating reverse-phase high-performance liquid chromatographic method was developed and validated for the analysis of apigenin and luteolin. The degradation behavior of apigenin and luteolin was investigated under different stress conditions as recommended by the International Conference on Harmonization (ICH). Methods: In the present study, a reversed-phase high-performance liquid chromatography method was developed and the resolution of the plant constituents was successfully achieved using Hibar Lichrospher C8 column with ultraviolet detector at a wavelength of 269 nm. The mobile phase consisted of methanol and 0.5% trifluoroacetic acid (80:20 v/v) at a flow rate of 1.0 ml/min. Both apigenin and luteolin were subjected to various stress degradation studies such as oxidation, acid and alkaline hydrolysis, and photolytic degradation. Results: The proposed method was found to be linear (1–5 μg/ml) with the linear correlation coefficient of R2=0.99. Although the degradation products of stressed conditions were not identified, the methods were able to detect the changes due to stress condition. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. Forced degradation studies on apigenin and luteolin give information about their storage and intrinsic stability conditions considering the advanced pharmaceutical aspects of formulations.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING REVERSE-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF SAQUINAVIR, RITONAVIR, AND AMPRENAVIR

2018 ◽  
Vol 11 (6) ◽  
pp. 390
Author(s):  
Mangamma Kuna ◽  
Gowri Sankar Dannana
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Array Detector ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Relative Standard ◽  
Liquid Chromatography Method

Objective: The objective of the study was to develop and validate a sensitive, precise, and accurate stability indicating reverse-phase (RP) high-performance liquid chromatography method for the quantification of saquinavir, ritonavir, and amprenavir simultaneously.Methods: The determination of saquinavir, ritonavir, and amprenavir in their mixtures was done using a mobile phase consisted of 0.1M phosphate buffer (pH 3.5) and methanol (70:30, v/v). The method is based on the simultaneous separation of studied drugs in a RP Inertsil ODS C18 (4.6 mm×100 mm, 5 μm) column at ambient temperature. Detection and quantitation were achieved with photodiode array detector set at 260 nm.Results: Saquinavir, ritonavir, and amprenavir showed linearity over a concentration range of 40–200 μg/ml (R2-0.9994), 20–100 μg/ml (R2-0.9992), and 30–150 μg/ml (R2-0.9990), respectively. The limit of quantification was 0.64 μg/ml, 0.57 μg/ml, and 0.53 μg/ml for saquinavir, ritonavir, and amprenavir, respectively. The accuracies for the three drugs were in the range of 99.40–100.53% (saquinavir), 99.45-100.47% (ritonavir), and 100.03–100.53% (amprenavir). The percentage relative standard deviations for the studied drugs were 0.785–0.848% (saquinavir), 0.338–0.499% (ritonavir), and 0.336–0.775% (amprenavir). No peaks were observed at the retention time of saquinavir, ritonavir, and amprenavir in placebo blank, mobile phase blank and stress degraded samples which suggested that the proposed was selective and specific.Conclusion: The method was found to be suitable for the regular analysis of saquinavir, ritonavir, and amprenavir simultaneously in the presence of their stress degradation products.Objective: The objective of the study was to develop and validate a sensitive, precise, and accurate stability indicating reverse-phase (RP) high-performance liquid chromatography method for the quantification of saquinavir, ritonavir, and amprenavir simultaneously. Methods: The determination of saquinavir, ritonavir, and amprenavir in their mixtures was done using a mobile phase consisted of 0.1M phosphate buffer (pH 3.5) and methanol (70:30, v/v). The method is based on the simultaneous separation of studied drugs in a RP Inertsil ODS C18 (4.6 mm×100 mm, 5 μm) column at ambient temperature. Detection and quantitation were achieved with photodiode array detector set at 260 nm. Results: Saquinavir, ritonavir, and amprenavir showed linearity over a concentration range of 40–200 μg/ml (R2-0.9994), 20–100 μg/ml (R2-0.9992), and 30–150 μg/ml (R2-0.9990), respectively. The limit of quantification was 0.64 μg/ml, 0.57 μg/ml, and 0.53 μg/ml for saquinavir, ritonavir, and amprenavir, respectively. The accuracies for the three drugs were in the range of 99.40–100.53% (saquinavir), 99.45-100.47% (ritonavir), and 100.03–100.53% (amprenavir). The percentage relative standard deviations for the studied drugs were 0.785–0.848% (saquinavir), 0.338–0.499% (ritonavir), and 0.336–0.775% (amprenavir). No peaks were observed at the retention time of saquinavir, ritonavir, and amprenavir in placebo blank, mobile phase blank and stress degraded samples which suggested that the proposed was selective and specific. Conclusion: The method was found to be suitable for the regular analysis of saquinavir, ritonavir, and amprenavir simultaneously in the presence of their stress degradation products.

scholarly journals A NEW NP-UPLC METHOD FOR THE SEPARATION AND SIMULTANEOUS QUANTIFICATION OF RAMUCIRUMAB AND ERLOTINIB

2021 ◽  
pp. 75-81
Author(s):  
SIVA MADHU CHAITANYA ◽  
SRINATH NISSANKARARAO ◽  
SATYA LAKSHMI GANDHAM
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Ultra Performance Liquid Chromatography ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Chiralcel Od ◽  
Successful Separation ◽  
Liquid Chromatography Method ◽  
Fine Resolution

Objective: This investigation demonstrates a stability-indicating and reliable “normal phase ultra-performance liquid chromatography” method to simultaneously quantify Ramucirumab and Erlotinib in the pharmaceutical dosage form. Methods: Successful separation was accomplished using Chiralcel-OD-3 column (50 mm x 4.6 mm, 3 μm) with an isocratic type of elution using a mobile phase containing n-hexane+isopropyl alcohol+methanol (89:10:1), respectively with 1.0 ml/min flow rate. The wavelength sensor was attuned at 266 nm to quantify Ramucirumab and Erlotinib. Results: Erlotinib and Ramucirumab peaks were eluted with fine resolution at retention times 1.7807 min and 3.175 min, respectively. In the 10-150 μg/ml and 1-15 μg/ml concentration ranges for Erlotinib and Ramucirumab, the calibration graphs were linear, with regression coefficients of 0.99928 and 0.99976, respectively. The suggested ultra-performance liquid chromatography approach has been shown as sensitive, precise, robust, accurate, specific and stability indicating through the resolution of Erlotinib and Ramucirumab from its degradation-based compounds. Conclusion: The established ultra-performance liquid chromatography technique was effectively extended to the evaluation of Erlotinib and Ramucirumab in the pharmaceutical dosage form and the test results appeared satisfactory.

scholarly journals SEPARATION AND ANALYSIS OF AMLODIPINE/BENAZEPRIL COMBINATION IN CAPSULES BY A NOVEL ION PAIR LIQUID CHROMATOGRAPHY

2019 ◽  
Vol 11 (1) ◽  
pp. 107 ◽  
Author(s):  
Saleh Trefi ◽  
Yaser Bitar
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
Degradation Products ◽  
Correlation Coefficients ◽  
Ion Pair ◽  
Chromatography Method ◽  
Relative Standard ◽  
Liquid Chromatography Method

Objective: The objective of this study was to develop and validate a novel ion-pair liquid chromatography method, in order to separate and assay of amlodipine/benazepril combination in capsules. This method was a fast, practical and additional choice in quality control laboratories.Methods: The chromatographic conditions comprised of a classical C18-type stationary phase (250 × 4.6 mm, 5μ), with a mobile phase consisting of: 45% of 10-3 M of cetrimide and 55% acetonitrile. The flow rate was 1 ml/min; the detection wavelength was at 242 nm, under ambient temperature.Results: The method was validated for linearity with correlation coefficients very close to one, the accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products and excipients.Conclusion: The results presented in this paper showed that the developed method was fast and applicable, for the separation and determination of amlodipine/benazepril combination in capsules.

scholarly journals A SIMPLE REVERSE PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF VALSARTAN IN BULK AND IT’S TABLET DOSAGE FORM

2017 ◽  
Vol 10 (12) ◽  
pp. 333
Author(s):  
Ramreddy Godela ◽  
Sherisha Bhavani
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Quantitative Determination ◽  
High Performance ◽  
Dosage Form ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Tablet Dosage

Objective: The most important objective of the present research work is to develop simple, specific, rapid, accurate, and sensitive reverse-phase high-performance liquid chromatography method and validated for the qualitative and quantitative determination of valsartan in its active pharmaceutical ingredient and tablet dosage form according to ICH guidelines.Proposed Method: An isocratic separation was done using Phenomenex C18 column possess 75×4.6 mm, 2.6 μ,100 A0 dimensions with mobile phase composition of water:acetonitrile (30:70% v/v) by maintaining 1 ml/minute flow rate and response detected at a wavelength of 247 nm.Results: The retention time of valsartan was found to be 2.71 minutes, limit of detection and limit of quantification were observed at 1.24 μg/ml and 3.6 μg/ml concentration, respectively, and a calibration curve was linear in the concentration range of 5-50 μg/ml with coefficient of correlation 0.99. The percentage recovery (accuracy) was in the range of 98.9-102%, and the % relative standard deviation was observed to be <2%.Conclusion: The proposed method was validated for accuracy, precision, sensitivity, linearity, and robustness and successfully employed for the quantitative determination of valsartan in tablet dosage form in quality control department of pharmaceutical industry.

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