【作者】 李冰； 刘拥军； 郭瑞臣；

【Author】 LI Bing 1, LIU Yong-jun2, GUO Rui-chen3 (1. Shandong Institute of Drug Control,Jinan 250012;2.Institute of Materia Medica, Shandong Academy of Medical Science 250062;3.Institute of Clinical Pharmacology, Qilu Hospital of Shandong Univewrsity, Jinan 250012)

【机构】 山东省药品检验所； 山东医学科学院药物研究所； 山东大学齐鲁医院临床药理研究所；

【摘要】 目的对中药制剂中掺入的盐酸二甲双胍、盐酸苯乙双胍、格列吡嗪、盐酸吡格列酮、格列齐特、格列本脲、格列美脲、格列喹酮成分进行鉴定。方法色谱柱为ZORBAXSB-C18(150×4.6mm,5μm),流动相:A甲醇(含1%冰醋酸):B甲酸盐缓冲溶液(20mmol·L-1甲酸铵溶液,用冰醋酸调节pH值至3.86)=70:30,保持10分钟,10～20分钟,A:70～90%,流速1ml·min-1,检测波长为240nm;大气压电喷雾电离源,正离子模式,雾化气压力30psi,干燥气温度350℃,流速10L·min-1,毛细管电压4000V,扫描范围100~600。结果检出7批样品中掺入的盐酸二甲双胍、盐酸苯乙双胍、格列齐特、格列本脲、格列美脲。结论建立的LC-MS/MS方法可同时筛选及鉴定中成药中掺入的上述降糖西药。更多还原

【Abstract】 OBJECTIVE To identify metformin hydrochlorid,phenformin hydrochloride,glipizide,pioglitazone hydrochloride,gliclazide, glibenclamide,glimepiride and gliquidone illegally-added into traditional Chinese medicine with a evaluated HPLC method. METHODS The column was ZORBAX SB- C18(150×4.6mm,5μm),the mobile phase A (1% acetate acid methanol solution,70%):B(20mmol·L-1ammonium formate buffer solution, adjusted pH to 3.86 with acetate acid, 30%) was held for 10 minutes, and then the mobile phase A was increased linearly to 90% within 10 minutes, and the flow rate was 1ml·min-1, the detection wavelength was at 240nm.Electrospray ionization source (ESI) was applied and operated in positive ion mode, nebulizer pressure was 30psi,drying gas temperature was at 350℃ and flow was 10L·min-1,the Vcap was set at 4000V,the scanning range was from 100 to 600. RESULTS The illegally-added metformin hydrochloride ,phenformin hydrochloride,gliclazide,glibenclamide,glimepiride were detected in seven analyzed samples. CONCLUSION The LC-MS/MS methods established can be used to identify and quantitatively determine the eight above mentioned components added into traditional Chinese medicine.更多还原