Lakshmi Karunanidhi S, Rajesh Tirumala
Department of Pharmaceutical Analysis, SRM College of Pharmacy, SRM University, Kattankulathur, Tamil Nadu 603203, India.
ISRN Pharm. 2011;2011:521353. doi: 10.5402/2011/521353. Epub 2011 Jul 12.
An analytical method based on isocratic reverse phase high-performance liquid chromatography was developed and validated for the separation and quantification of eight antidiabetic drugs: rosiglitazone, pioglitazone, glipizide, gliclazide, repaglinide, nateglinide, glibenclamide, and glimepiride for their application in human plasma assay. Metformin is used as internal standard. Analysis was done on Onyx monolithic C(18) column (100 × 4.6 mm, i.d., 5 μm) using a mixture of 0.05% formic acid in water and methanol in the ratio of 42 : 58 (v/v) fixed at a flow rate of 0.5 mL/min, and they were monitored at 234 nm. Separation was achieved in less than 20 min. The calibration curves were linear in the range of 50-2000 ng/mL. The method was validated for its recovery, intra- and interday precision, stability, specificity, and selectivity. Plasma samples were prepared using solid-phase extraction of analytes. Hence, the developed method was found to be suitable for the routine analysis of selected antidiabetic drugs in biological matrices.
建立了一种基于等度反相高效液相色谱的分析方法,并对其进行了验证,用于分离和定量测定罗格列酮、吡格列酮、格列吡嗪、格列齐特、瑞格列奈、那格列奈、格列本脲和格列美脲这八种抗糖尿病药物,以用于人体血浆分析。二甲双胍用作内标。采用Onyx整体式C(18)柱(100×4.6 mm,内径,5 μm)进行分析,使用0.05%甲酸水溶液和甲醇按42 : 58 (v/v)的比例混合,流速固定为0.5 mL/min,并在234 nm波长处进行监测。在不到20 分钟内实现了分离。校准曲线在50 - 2000 ng/mL范围内呈线性。该方法在回收率、日内和日间精密度、稳定性、特异性和选择性方面均得到验证。血浆样品采用分析物固相萃取法制备。因此,所建立的方法适用于生物基质中所选抗糖尿病药物的常规分析。