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药物和人血清中二甲双胍、雷尼替丁和法莫替丁的 GC 分析。

GC Analysis of Metformin, Ranitidine and Famotidine from Pharmaceuticals and Human Serum.

机构信息

Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro 76080, Sindh, Pakistan.

Dr. M.A. Kazi Institute of Chemistry, University of Sindh, Jamshoro 76080, Sindh, Pakistan.

出版信息

J Chromatogr Sci. 2023 Nov 5;61(9):807-813. doi: 10.1093/chromsci/bmad047.

Abstract

A method has been designed based on gas chromatography with flame ionization detection (FID) for the separation and analyses of ranitidine, famotidine and metformin after pre-column derivatization with trifluoroacetylacetone and ethyl chloroformate. DB-1 (30 m × 0.32 mm id) column with film thickness 0.25 μm was used for the separation at an initial temperature of column was 100°C for 2 min, and ramping at 20°C/min up to 250°C, with a hold time of 3 min. The rate of nitrogen flow was 2.5 mL/min and FID was used for detection. Complete separation was obtained between all the three drugs including excess of derivatization reagents. Linear calibration curves and detection limits were obtained in the ranges 0.1-30 μg/mL and 0.011-0.015 μg/mL. The procedure was repeatable in terms of peak heights/peak areas and retention time (n = 5) for derivatization, quantitation and separation with relative standard deviations (RSDs) within 2.0-3.0%. The approach was examined for the analyses of drug products and serum after the intake of the drugs by healthy volunteers, and recoveries were obtained within 95-98% with RSDs 2.4-3.1%.

摘要

一种基于气相色谱法与火焰离子化检测(FID)的方法已经被设计出来,用于对雷尼替丁、法莫替丁和二甲双胍进行分离和分析,这些药物在进行柱前衍生化时,使用了三氟乙酰丙酮和氯甲酸乙酯。采用 DB-1(30 m×0.32 mm id)柱,膜厚 0.25 μm,在初始柱温为 100°C 的条件下进行分离,以 20°C/min 的速度升温至 250°C,保持 3 min。氮气流速为 2.5 mL/min,FID 用于检测。所有三种药物(包括过量的衍生化试剂)都得到了完全分离。在线性范围内(0.1-30 μg/mL)和检测限范围内(0.011-0.015 μg/mL),均获得了线性校准曲线和检测限。在衍生化、定量和分离方面,该程序在峰高/峰面积和保留时间方面具有可重复性(n=5),相对标准偏差(RSD)在 2.0-3.0%以内。该方法已用于健康志愿者服用药物后的药物制剂和血清分析,回收率在 95-98%之间,RSD 为 2.4-3.1%。

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