Importance of mobile phase and injection solvent selection during rapid method development and sample analysis in drug discovery bioanalysis illustrated using convenient multiplexed LC-MS/MS

2010 ◽  
Vol 2 (4) ◽  
pp. 375 ◽  
Author(s):  
Jian Wang ◽  
Anne-Francoise Aubry ◽  
Georgia Cornelius ◽  
Christian Caporuscio ◽  
Bogdan Sleczka ◽  
...  
Keyword(s):  
Drug Discovery ◽  
Rapid Method ◽  
Mobile Phase ◽  
Method Development ◽  
Sample Analysis ◽  
Solvent Selection

FORCED INDICATING UPLC-DAD METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF APALUTAMIDE IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (09) ◽  
pp. 73-75
Author(s):  
China Babu D ◽  
Madhusudhana Chetty C ◽  
Mastanamma S. K ◽  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Uv Light ◽  
Accurate Method ◽  
Pharmaceutical Dosage Form ◽  
Good Ability ◽  
Acquity Uplc ◽  
Development And Validation

A new analytical method was developed for the estimation of apalutamide in bulk and its pharmaceutical formulation. The sensitive, précise and accurate method was developed by using Waters Acquity UPLC system equipped with quaternary gradient pump. The column used was Waters C18 150 X 2.1 mm X 1.7 µm and mobile phase was 0.2 % OPA buffer in water : acetonitrile in the ratio of 25:75 V/V. The buffer pH was maintained at 4.5. The fl ow rate of mobile phase was 0.5 mL min-1 and detection was at 272 nm by using PDA detector. The method was performed at ambient temperature. The retention time of the apalutamide was 1.27 min. The % RSD value in precision was >2 %. The accuracy of the method was found to be between 99.54 % - 100.01 %. The limit of detection and limit of quantifi cation values were found to be 0.14 µg mL-1 and 0.48 µg mL-1, respectively. The linearity concentration range was found to be 11.25 - 67.5 µg mL-1, it show wide linearity concentration range. The method was proved to have good robustness after changing parameters of fl ow rate, temperature and mobile phase composition. The method showed good ability towards different stress conditions of acidity, alkalinity, peroxide and UV-light. The method can be used for the routine analysis of apalutamide in bulk and its pharmaceutical dosage form by using UPLC.

RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF AMPHOTERICIN B

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
Author(s):  
L Mohankrishna ◽  
◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya
Keyword(s):  
Amphotericin B ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Phase Combination ◽  
Hplc Method Development

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

scholarly journals RP-HPLC Method Development and Validation for Cleaning Residue Determination of Tofacitinib Citrate in Tofacitinib Tablets

2021 ◽  
pp. 262-276
Author(s):  
Thaticherla Kaleswararao ◽  
Duvvuri Suryakala
Keyword(s):  
Method Development ◽  
Drug Product ◽  
Hplc Method ◽  
Solution Stability ◽  
Sample Analysis ◽  
Validation Data ◽  
Manufacturing Equipment ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Development And Validation

A novel, Specific, and precise RP-HPLC method was developed to determine the residue content of Tofacitinib citrate left on the surface of equipment used in the manufacturing process. The manufacturing equipment considered in assessment of cleaning has been verified and found the tools assembled to the equipment are made up of Stainless steel, Glass, Teflon and plastic. Hence, these surfaces of manufacturing equipment that come in contact with the drug product during manufacturing are considered for evaluation of the cleaning procedure. By developing and validating an analytical method for residue estimation, the manufacturing equipment can be evaluated for efficient cleaning and to release the manufacturing equipment for further intended use by minimizing the cross contaminations. The stationary phase suited for the well separation of components is CAPCELL PAK C18 150 x 4.6 mm, 3 μm; 0.4 % perchloric acid and acetonitrile in the ratio of 85:15 % v/v is the mobile phase pumped at a flow rate of 1.2 mL/min through the column at temperature of 40 ºC. Each run extended for 10 min as the Tofacitinib peak elutes at RT of 5.2 min. The method has been validated successfully for Specificity, Precision, Linearity, Accuracy, Ruggedness and Filter validation of both rinse and swab methods. The LOD, LOQ concentrations found to be 0.006, 0.019 µg/mL for swab method and 0.03 and 0.1 µg/mL for rinse method respectively. The correlation coefficient is 0.999 and method found linear from LOQ to 500% for swab method and LOQ to 200% for rinse method. Solution stability has been established to ensure the test solution get tested within the stable time (4 Days). Based on the filter validation data, it is concluded that PVDF filter is not suitable for cleaning sample analysis and 2 mL sample should be discarded when 0.45 µm Nylon filter is used for cleaning sample analysis.

scholarly journals Rapid LC/MS/MS Method Development for Drug Discovery

2005 ◽  
Vol 77 (19) ◽  
pp. 389 A-394 A ◽  
Author(s):  
Xiaoying Xu ◽  
Jing Lan ◽  
Walter A. Korfmacher
Keyword(s):  
Drug Discovery ◽  
Method Development

ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 66-68
Author(s):  
◽  
A. P Jadhav
Keyword(s):  
Immune Response ◽  
Ethyl Acetate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Marker Compounds ◽  
Hptlc Method

Talekt capsule is a branded polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively were used as marker compounds for developing a simple, accurate, precise and robust HPTLC method for simultaneous estimation. The mobile phase of toluene: ethyl acetate: formic acid (6.5: 3: 0.2 v/v/v) was used for separation. 381nm was used as wavelength for analysis. The Rf value obtained for curcumin, and embelin was found to be 0.51 ± 0.2 and 0.33 ± 0.2, respectively. The developed method was validated on the basis of ICH Q2 (R1) guidelines.

scholarly journals RP-HPLC Method Development and Its Validation for Quantitative Determination of Rimonabant in Human Plasma

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Shravan Bankey ◽  
Ganesh Tapadiya ◽  
Jasvant Lamale ◽  
Deepti Jain ◽  
Shweta Saboo ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Hplc Method Development

A simple, accurate, and precise HPLC method was developed and validated for determination of rimonabant in human plasma. Following liquid-liquid extraction, chromatographic separation was accomplished using C18 column with mobile phase consisting of acetonitrile : water (90 : 10, v/v), drug was detected at 260 nm using UVdetector. The LOD and LOQ were 3.0 and 10.0 μg/L, respectively. The method is linear in the interval 50.0–1000.0 μg/L. The average extraction recovery of drug from plasma was found to be 92.2%. The percent CV of the method was found to be less than 10.8%, and accuracy was found between 94.5 and 106.7%. The assay may be applied to a pharmacokinetic and bioequivalence study of rimonabant.

Sign in / Sign up

Export Citation Format

Share Document