scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF METOPROLOL AND ATORVASTATIN BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN ITS BULK AND PHARMACEUTICAL TABLET DOSAGE FORM USING BIORELEVANT DISSOLUTION MEDIA (FASTED STATE SMALL INTESTINAL FLUID)

2018 ◽  
Vol 11 ◽  
Author(s):  
Palani Shanmugasundaram ◽  
Kamarapu Sk2
Keyword(s):  
High Performance ◽  
Method Development ◽  
Reversed Phase ◽  
Biorelevant Dissolution ◽  
Fasted State ◽  
Method Development And Validation ◽  
Small Intestinal ◽  
Development And Validation ◽  
Biorelevant Dissolution Media

Objective: A present investigation is based on method development and validation for the simultaneous determination of metoprolol and atorvastatin by reversed-phase high-performance liquid chromatography in its bulk and pharmaceutical dosage form using a biorelevant dissolution media (fasted state small intestinal fluid). Methods: The chromatographic separation technique performed by an isocratic method for this column used Inertsil ODS-3 (4.6×150 mm, 5 μm). The ratio of mobile phase used is phosphate buffer 4.8 pH: acetonitrile (35:65v/v), flow rate 1 ml/min, and analysis time 15.0 min, UV detection was at 244 nm. Results: According to the International Conference on Harmonisation Q2 (R1) guidelines, the method validation was done. Peaks were observed at 2.227 min and 5.819 min, concentration range of linearity was obtained at 50–250 μg/ml and 10–50 μg/ml, linearity correlation coefficients were 0.9997 and 0.9995, limit of detection was 0.33 mg/ml and 0.21 mg/ml, and limit of quantification was 1.08 mg/ml and 0.69 mg/ml for metoprolol and atorvastatin, respectively. Conclusion: The obtained results for this method validation are within acceptance criteria. This method was more economical and stable for routine analysis.

Simultaneous method development and Validation by HPLC for Capecitabine and Oxaliplatin in mucoadhesive microspheres containing capsules

2021 ◽  
pp. 3365-3370
Author(s):  
Krishna Patel ◽  
Dipti Patel
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Dipotassium Hydrogen Phosphate ◽  
Liquid Chromatographic Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, specific and accurate reversed-phase high performance liquid chromatographic method was developed for the simultaneous determination of Capecitabine and Oxaliplatin, using a Hypersil BDS C18, 150x4.6 mm, 5μ column and a mobile phase composed of 10mM dipotassium hydrogen phosphate+0.1% TEA pH 5.0: Acetonitrile (50:50%v/v). The flow rate was 1.0 ml/min, and the detection wavelength was 245 nm. The injection volume was 20 μL. The retention times of Capecitabine and Oxaliplatin found 4.29 min and 5.52 min, respectively. Linearity was established for Capecitabine and Oxaliplatin in the range of 60-210μg/ml and 20-70 μg/ml, respectively. The percentage recoveries of Capecitabine and Oxaliplatin found to be in the range of 99.1-101.5% and 97.9-99.7 %, respectively. The proposed method validated for precision, accuracy, linearity range, and robustness. This method can successfully be employed for simultaneous quantitative analysis of Capecitabine and Oxaliplatin in the capsule.

Method Development and Validation of Propofol by Reverse Phase HPLC and its Estimation in Commercial Formulation

2021 ◽  
pp. 3139-3142
Author(s):  
Kuntal Mukherjee ◽  
S. T. Narenderan ◽  
B. Babu ◽  
Survi Mishra ◽  
S. N. Meyyanathan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase Hplc ◽  
Liquid Chromatographic Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, sensitive and rapid high performance liquid chromatographic method has been developed for the determination of Propofol. The main focus of the method was to determine Propofol in solution form as well as in marketed formulation. Chromatographic separation was achieved on Inertsil ODS-3V column (250mm x 4.6mm; 5µm) with a mobile phase consisting of methanol: water (85:15), with a flow rate of 1.0ml/min (UV detection at 270nm). Linearity was observed over the concentration range of 10-110µg/ml with a regression equation y=88048x + 44524 and having a regression value (R2) of 0.999. The LOD and LOQ values found to be 10ng and 100ng, respectively. No changes found in ruggedness and robustness studies. The percentage of recovery was found to be 95.25% to 101.81%. Validation studies revealed that the method was specific, accurate, precise, reliable, robust, reproducible and suitable for the quantitative analysis in its pharmaceutical formulations.

BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR SIMULANEOUS ESTIMATION OF NITAZOXANIDE AND OFLOXACIN IN HUMAN PLASMA BY RP-HPLC

INDIAN DRUGS ◽  
2021 ◽  
Vol 57 (10) ◽  
pp. 47-57
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Reversed Phase ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Lower Limits

An isocratic Reversed-Phase High Performance Liquid Chromatography method has been developed for rapid and simultaneous separation and estimation of two antibiotics, namely, nitazoxanide and ofloxacin, in human plasma. Separation was carried out on Altima C8 (150 x 4.6 mm, 5µ) column using a mobile phase of 0.1% ortho phosphoric acid: acetonitrile (50:50, V/V) at 260 nm. The retention time of nitazoxanide and ofloxacin was noted to be 4.850 and 7.949 min, respectively. The average % recovery for nitazoxanide and ofloxacin were 98.012 % and 94.176 %, respectively and reproducibility was found to be satisfactory. The linearity was investigated in the concentration range of 0.02-2 µg/ml (r2=0.9996) for nitazoxanide and 0.008-0.8 µg/ml (r2=0.9998) for ofloxacin. The lower limits of quantification were 0.0196 µg/ml and 0.0079 µg/ml for nitazoxanide and ofloxacin, respectively, which reach the level of both drugs possibly found in human plasma. The proposed method can be applied for etermination of nitazoxanide and ofloxacin from dosage forms during pharmacokinetic study.

scholarly journals HPTLC Method Development and Validation for Determination of Rutin in Flavanoidal Fraction ofHibiscus micranthusLinn.

2011 ◽  
Vol 8 (3) ◽  
pp. 1444-1450 ◽  
Author(s):  
K. Ashok Kumar ◽  
S. Ramachandra Shetty ◽  
Laxmi Narasu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Methanolic Extract ◽  
Method Development And Validation ◽  
Stem Extract ◽  
Acetic Acid Water ◽  
Flavonoid Fraction ◽  
Development And Validation ◽  
Hptlc Method

A simple, precise and accurate high-performance thin-layer chromatographic method has been established for the determination of rutin in the stem extract ofHibiscus micranthusLinn. A flavonoid fraction of methanolic extract of the stem powder was used for the experimental work. Separation was performed on silica gel 60 F254HPTLC plates withn-butanol: acetic acid: water: ammonia 3:1:1:1(v/v), as mobile phase. The determination was carried out using the densitometric absorbance mode at 286 nm. Rutin response was linear over the range 50–400 ng/μL. The concentration of rutin in the flavanoidal fraction was found to be 9.93%. The HPTLC method was evaluated in terms of sensitivity, accuracy, precision and reproducibility.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF EPROSARTAN MESYLATE AND ITS IMPURITIES USING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 8 (4) ◽  
pp. 49 ◽  
Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase ◽  
Related Substances ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.

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