Zhou Si, Zuo Pengxiao, Zuo Yuegang, Deng Yiwei
Department of Chemistry and Biochemistry, University of Massachusetts Dartmouth, 285 Old Westport Road, North Dartmouth, MA 02747, USA.
Department of Natural Sciences, University of Michigan, Dearborn, MI 48128, USA.
Saudi Pharm J. 2017 Sep;25(6):852-856. doi: 10.1016/j.jsps.2017.01.002. Epub 2017 Jan 25.
Glimepiride is one of the most widely prescribed antidiabetic drugs and contains both hydrophobic and hydrophilic functional groups in its molecules, and thus could be analyzed by either reversed-phase high performance liquid chromatography (HPLC) or hydrophilic interaction liquid chromatography (HILIC). In the literature, however, only reversed-phase HPLC has been reported. In this study, a simple, rapid and accurate hydrophilic interaction liquid chromatographic method was developed for the determination of glimepiride in pharmaceutical formulations. The analytical method comprised a fast ultrasound-assisted extraction with acetonitrile as a solvent followed by HILIC separation and quantification using a Waters Spherisorb SNH hydrophilic column with a mobile phase consisting of acetonitrile and aqueous acetate buffer (5.0 mM). The retention time of glimepiride increased slightly with decrease of mobile phase pH value from 6.8 to 5.8 and of acetonitrile content from 60% to 40%, indicating that both hydrophilic, ionic, and hydrophobic interactions were involved in the HILIC retention and elution mechanisms. Quantitation was carried out with a mobile phase of 40% acetonitrile and 60% aqueous acetate buffer (5.0 mM) at pH 6.3, by relating the peak area of glimepiride to that of the internal standard, with a detection limit of 15.0 μg/L. UV light absorption responses at 228 nm were linear over a wide concentration range from 50.0 μg/L to 6.00 mg/L. The recoveries of the standard added to pharmaceutical tablet samples were 99.4-103.0% for glimepiride, and the relative standard deviation for the analyte was less than 1.0%. This method has been successfully applied to determine the glimepiride contents in pharmaceutical formulations.
格列美脲是处方量最大的抗糖尿病药物之一，其分子中同时含有疏水和亲水官能团，因此既可以通过反相高效液相色谱法（HPLC）分析，也可以通过亲水作用液相色谱法（HILIC）分析。然而，文献中仅报道了反相HPLC法。本研究建立了一种简单、快速且准确的亲水作用液相色谱法，用于测定药物制剂中的格列美脲。该分析方法包括以乙腈为溶剂的快速超声辅助萃取，然后使用Waters Spherisorb SNH亲水柱进行HILIC分离和定量，流动相由乙腈和乙酸盐水溶液缓冲液（5.0 mM）组成。随着流动相pH值从6.8降至5.8以及乙腈含量从60%降至40%，格列美脲的保留时间略有增加，这表明亲水、离子和疏水相互作用均参与了HILIC保留和洗脱机制。在pH 6.3时，采用40%乙腈和60%乙酸盐水溶液缓冲液（5.0 mM）的流动相，通过将格列美脲的峰面积与内标峰面积相关联进行定量，检测限为15.0 μg/L。在50.0 μg/L至6.00 mg/L的宽浓度范围内，228 nm处的紫外光吸收响应呈线性。添加到药物片剂样品中的格列美脲标准回收率为99.4 - 103.0%，分析物的相对标准偏差小于1.0%。该方法已成功应用于测定药物制剂中格列美脲的含量。
