Method For Determination Of Glibenclamide Research Articles

Rapid, Validated UPLC-MS/MS Method for Determination of Glibenclamide in Rat Plasma.

Quick and specific bioanalytical methods are required for analyzing drugs in biological samples. A simple, quick, sensitive, and specific UPLC-MS/MS method was developed and validated for glibenclamide determination in plasma samples. The plasma samples were processed by protein precipitation technique. Glimepiride was used as internal standard (IS). Glibenclamide and glimepiride were eluted on C18 column (Acquity UPLC®BEH). Mobile phase consisting of acetonitrile (0.1% formic acid) and water (0.1% formic acid) was pumped in binary gradient mode at flow rate of 150 μL/min. Glibenclamide and IS elution time was about 1.0 min, and total run time was 2.0 min. The mass spectrometer (triple-quadrupole) was operated in positive electrospray ionization mode. Sodium adducts [M + Na]+ of glibenclamide and IS were monitored in MRM mode. A linear calibration curve was obtained in the range of 10-1280 ng/mL, with regression equation Y = 0.0076 X – 0.0165 and linear regression coefficient r2 = 0.999. Lower limit of quantitation was 10 ng/mL. Accuracy of the method at LQC, MQC, and HQC was 109.7% (± 6.7), 93.6% (± 0.4), and 99.3% (± 1.9), respectively. The coefficient of variation for precision at all QC concentrations was less than 6%. Recovery at LLQC, MQC, and HQC was 104.2% (± 4.9), 100.6% (± 0.9), and 102.9% (± 5.8), respectively. The method was successfully implemented for pharmacokinetic investigations (in-house data).

Dissolution test for glibenclamide tablets

The aim of this work is to develop and validate a dissolution test for glibenclamide tablets. Optimal conditions to carry out the dissolution test are 500 mL of phosphate buffer at pH 8.0, paddles at 75 rpm stirring speed, time test set to 60 min and using equipment with six vessels. The derivative UV spectrophotometric method for determination of glibenclamide released was developed, validated and compared with the HPLC method. The UVDS method presents linearity (r² = 0.9999) in the concentration range of 5-14 µg/mL. Precision and recoveries were 0.42% and 100.25%, respectively. The method was applied to three products commercially available on the Brazilian market.

High-Performance Liquid Chromatographic Method for Determination of Glibenclamide in Human Plasma

Abstract An HPLC method for quantitative determination of glibenclamide in human plasma is described. The methodology is based on simple one step extraction of glibenclamide and diazepam (internal standard) from human plasma with dichloromethane. The drugs were eluted from a resolve 5 u spherical C18 column with a mobile phase consisting of 0.05 M ammonium dihydrogen phosphate:methanol (40:60%, v/v) adjusted to pH 4.0 with phosphoric acid. The drug and the internal standard were eluted at a flow rate of 1.2 ml per minute, and the optimum detector wavelength was 230 nm. The chromatography time was eleven minutes and the resolution between the drug and internal standard was excellent. Quantitation was achieved by the measurement of peak area ratios and the minimum detectable concentration was 5 ng/ml. The calibration curve of the assay was linear over the range of 10–400 ng/ml. The intraday coefficient of variation were ranged from 0.53% to 3.19%, whereas interday coefficient of variation were from 2.31% to...