固相萃取-高效液相色谱测定降糖汤药中的盐酸二甲双胍含量  

Determination of metformin hydrochloride added in anti-diabetic herbal medicine by HPLC using SPE

作　　者：杨小秋[1] 邱燕菊 胡思前[1] 万昆[1] 宋春宇[2] 

机构地区：[1]江汉大学光电化学材料与器件省部共建教育部重点实验室,武汉430056 [2]武汉市中心医院内分泌科,武汉430014

出　　处：《分析试验室》2015年第12期1392-1394,共3页Chinese Journal of Analysis Laboratory

基　　金：武汉市科技攻关项目(2014022905011274)资助

摘　　要：建立了固相萃取-高效液相色谱测定降糖汤药中化学添加成分盐酸二甲双胍的方法。降糖汤药样品经乙醇涡旋超声提取后,使用弱阳离子固相萃取小柱净化后进样,使用Lnertsil ODS-3 C18(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈:甲醇:0.02 mol/L乙酸铵=20:20:60(V/V/V),流速0.4 m L/min,柱温30℃,紫外检测波长237 nm,外标法定量。标准曲线的线性范围在2.5~200 mg/L之间,相关系数r^2=0.9998,方法检出限为0.04 mg/L,加标回收率为89.5%~93.9%,RSD为5.3%。方法适用于降糖汤药中盐酸二甲双胍非法添加量的测定。A method was developed for the determination of metformin hydrochloride added in anti-diabetic herbal medicine by high performance liquid chromatography using solid phase extraction. The metformin hydrochloride was extracted by ethanol using ultrasonic after curling by vortex separator, then the extract was cleaned up by weak cation extraction column and was detected by HPLC in the optimal chromatography condition. The HPLC column of Lnertsil ODS-3 C18 （4.6mm Х 250mm, 5μm） was used with elution （0.4 mL/min） by acetonitrile-methanol-0.02 mol/L acetic acid ammonia （20： 20： 60, V/V/V） and the detection wavelength of HPLC was 237nm. A series of standard working solution was prepared for the quantification of the sample, the standard curve equation was Y = 3. 7801X ＋ 1. 9225 and the correlation coefficient r^2 = 0. 9998 with concentration ranging from 2.5 mg/L to 200 mg/L. The limit of detection was 0.04 mg/L and the recovery rate ranged from 89.5% to 93.9% and the RSD was less than 5.3%. This method was easy to operate and had good accuracy and could be used to supervise the herbal medicine market and confirm the medicine quality.

关 键 词：固相萃取 高效液相色谱 降糖汤药 盐酸二甲双胍 

分 类 号：TQ460.7[化学工程—制药化工]