辅助降糖胶囊中3种双胍类物质的快速筛查

Rapid screening of three kinds of guanidine contraband in auxiliary sugar reduction capsule

建立并验证了反相离子对—液质联用法对于辅助降糖胶囊中3种双胍类物质盐酸二甲双胍、盐酸苯乙双胍、盐酸丁二胍进行快速筛查及定性定量检测的方法。以甲醇为样品提取溶剂,超声辅助萃取,选用安捷伦C_(18)(4.6×250 mm,5μm)色谱柱,检测波长235nm,以甲醇—乙酸铵溶液(0.01mol/L)为流动相进行梯度洗脱,流速0.5mL/min,进样量5μL。液相色谱检测后,进入质谱仪进行正离子模式扫描筛查。该分析方法下,加标回收率为87.5%~108.4%,相对标准偏差为0.5%~7.4%,精密度和准确度良好。

A method for rapid screening and qualitative and quantitative determination of three biguanides,MH,PH and BH,in Jiangtang capsules by reversed-phase ion-pair-LC-MS was established and validated.Anagilent technologies C18 column(4.6×250 mm,5μm)was used for the determination at 235 nm.A methanol-B ammonium acetate solution(0.01 mol/L)was used as the mobile phase for gradient elution at a flow rate of 0.5 mL/min.After the HPLC detection,the mass spectrometer for positive ion mode scanning was used for screening.The recovery of standard addition was 87.5%~108.4%,and the relative standard deviation was 0.5%~7.4%,with good precision and accuracy.