Salem Hesham
Minia University, Faculty of Pharmacy, Analytical Chemistry Department, Minia, Egypt.
J AOAC Int. 2010 Jan-Feb;93(1):133-40.
Three methods were developed for simultaneous determination of metformin hydrochloride and glyburide in an antihyperglycemic binary mixture without previous separation. In the first method, a reversed-phase HPLC column with acetonitrile-water (60 + 40, v/v) mobile phase at 0.9 mL/min flow rate was used to separate both compounds, with UV detection at 254 nm. Linearity was obtained in the concentration range of 0.06--0.24 microg/mL for glyburide and 1.5-6.0 microg/mL for metformin hydrochloride. The second method depended on first- and second-derivative UV spectrometry with zero-crossing measurements. The first-derivative amplitude at 261 nm was selected for the assay of glyburide, and the second-derivative amplitude at 235 nm was selected for the assay of metformin hydrochloride. The third method depended on measuring the first derivative of the ratio-spectra at 241 nm for glyburide and 227 nm for metformin hydrochloride. For the second and third methods, Beer's law was obeyed in the range of 10-55 microg/mL for glyburide and 20-200 microg/mL for metformin. The proposed methods were extensively validated and applied for the analysis of some pharmaceutical formulations containing binary mixtures of the mentioned drugs.
开发了三种无需预先分离即可同时测定降血糖二元混合物中盐酸二甲双胍和格列本脲的方法。第一种方法使用反相高效液相色谱柱，以乙腈 - 水（60 + 40，v/v）为流动相，流速为0.9 mL/min来分离两种化合物，在254 nm处进行紫外检测。格列本脲在0.06 - 0.24 μg/mL浓度范围内以及盐酸二甲双胍在1.5 - 6.0 μg/mL浓度范围内呈线性关系。第二种方法基于一阶和二阶导数紫外光谱法及零交叉测量。选择261 nm处的一阶导数幅度用于测定格列本脲，选择235 nm处的二阶导数幅度用于测定盐酸二甲双胍。第三种方法基于测量241 nm处格列本脲和227 nm处盐酸二甲双胍的比率光谱的一阶导数。对于第二种和第三种方法，格列本脲在10 - 55 μg/mL范围内以及盐酸二甲双胍在20 - 200 μg/mL范围内符合比尔定律。所提出的方法经过广泛验证，并应用于分析含有上述药物二元混合物的一些药物制剂。
