Department of Microbiology, Faculty of Science, University of Karachi, Karachi 75270, Pakistan.
J Anal Methods Chem. 2013;2013:297285. doi: 10.1155/2013/297285. Epub 2013 Oct 27.
A reverse phase stability indicating HPLC method for simultaneous determination of two antispasmodic drugs in pharmaceutical parenteral dosage forms (injectable) and in serum has been developed and validated. Mobile phase ingredients consist of Acetonitrile : buffer : sulfuric acid 0.1 M (50 : 50 : 0.3 v/v/v), at flow rate 1.0 mL/min using a Hibar μ Bondapak ODS C18 column monitored at dual wavelength of 266 nm and 205 nm for phloroglucinol and trimethylphloroglucinol, respectively. The drugs were subjected to stress conditions of hydrolysis (oxidation, base, acid, and thermal degradation). Oxidation degraded the molecule drastically while there was not so much significant effect of other stress conditions. The calibration curve was linear with a correlation coefficient of 0.9999 and 0.9992 for PG and TMP, respectively. The drug recoveries fall in the range of 98.56% and 101.24% with 10 pg/mL and 33 pg/mL limit of detection and limit of quantification for both phloroglucinol and trimethylphloroglucinol. The method was validated in accordance with ICH guidelines and was applied successfully to quantify the amount of trimethylphloroglucinol and phloroglucinol in bulk, injectable form and physiological fluid. Forced degradation studies proved the stability indicating abilities of the method.
已开发和验证了一种反相稳定指示 HPLC 方法，用于同时测定药物注射剂型（注射液）和血清中的两种抗痉挛药物。流动相成分由乙腈：缓冲液：硫酸 0.1 M（50：50：0.3 v/v/v）组成，流速为 1.0 mL/min，使用 Hibar μ Bondapak ODS C18 柱，在 266nm 和 205nm 处分别监测 phloroglucinol 和 trimethylphloroglucinol 的双波长。药物经受了水解（氧化、碱、酸和热降解）的应激条件。氧化使分子严重降解，而其他应激条件的影响不大。PG 和 TMP 的校准曲线均呈线性，相关系数分别为 0.9999 和 0.9992。药物回收率在 98.56%和 101.24%范围内，检测限和定量限分别为 10 pg/mL 和 33 pg/mL，适用于 phloroglucinol 和 trimethylphloroglucinol 的定量。该方法按照 ICH 指南进行了验证，并成功应用于批量、注射液和生理液中 trimethylphloroglucinol 和 phloroglucinol 的定量。强制降解研究证明了该方法的稳定性指示能力。
