Arayne M Saeed, Sultana Najma, Mirza Agha Zeeshan
Lab 9, Department of Chemistry, University of Karachi, Karachi.75270, Pakistan.
J Chromatogr Sci. 2011 Feb;49(2):114-7. doi: 10.1093/chrsci/49.2.114.
In the present study, a reverse-phase high performance liquid chromatography method was developed, validated and applied for the simultaneous determination of gliquidone, pioglitazone hydrochloride and verapamil in tablets and human serum. Chromatographic separation was achieved on a C18 column (5 μm, 25 × 0.46 cm) with a mobile phase consisting of methanol-water-acetonitrile (80:10:10 v/v/v) with a flow rate of 0.7 mL/min and pH adjusted to 3.50 with phosphoric acid at 230 nm. Glibenclamide was used as internal standard. The experimentally derived limit of detection and limit of quantitation were determined to be 0.24, 0.93, 0.40, and 0.80, 3.11, 1.36 μg/mL for gliquidone, pioglitazone, and verapamil, respectively. There were no interfering peaks due to the excipients present in the pharmaceutical tablets. Thus, the proposed method is simple and suitable for the simultaneous analysis of active ingredients in dosage forms and human serum.
在本研究中,开发、验证并应用了一种反相高效液相色谱法,用于同时测定片剂和人血清中的格列喹酮、盐酸吡格列酮和维拉帕米。在C18柱(5μm,25×0.46cm)上进行色谱分离,流动相由甲醇 - 水 - 乙腈(80:10:10 v/v/v)组成,流速为0.7 mL/min,用磷酸将pH调至3.50,检测波长为230nm。用格列本脲作为内标。实验得出的格列喹酮、吡格列酮和维拉帕米的检测限分别为0.24、0.93、0.40μg/mL,定量限分别为0.80、3.11、1.36μg/mL。药物片剂中的辅料没有干扰峰。因此,所提出的方法简单,适用于剂型和人血清中活性成分的同时分析。