液相色谱-质谱联用法检测2种中药降糖制剂中非法掺入的二甲双胍、苯乙双胍、格列吡嗪、格列本脲  

LC-MS determination of metformin,phenformin,glipizide and glyburide illegally mixed into two kind of antidiabetic Preparations of Traditional Chinese medicine

作　　者：刘福艳 谢元超 刘福强 王文笙 刘广桢 

机构地区：[1]山东省药品检验所,济南250101 [2]山东省邹城市中心店镇食品药品监督管理站,邹城273512 [3]山东鲁抗医药股份有限公司,济宁272021

出　　处：《药物分析杂志》2009年第3期440-444,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立检测降糖类中成药中非法掺入化学合成降糖药的专属性方法。方法:采用液相色谱-电喷雾质谱联用法。液相色谱:色谱柱为Agilent C18柱(150mm×4.6mm,5μm),流动相A为乙腈;流动相B为0.02mol·L-1醋酸铵(1000mL含冰醋酸1.0mL);流动相C为甲醇,梯度洗脱,流速0.4mL.min-1;柱温25℃。质谱:电喷雾电离源(ESI)正离子检测;质荷比范围m/z40～600,干燥气温度350℃;干燥气流速10L·min-1,;干燥气压力276kPa;源电压为5kV。通过相对分子质量、一级、二级质谱碎片信息、液相色谱保留时间和紫外光谱四方面的信息,对降糖类中成药的提取液进行定性鉴别和定量测定。结果:3批降糖类中成药,1批被检测到同时掺有二甲双胍和格列本脲,1批被检测到同时掺有苯乙双胍和格列本脲,1批未检出。结论:该方法选择性强,灵敏度高,可作为分析中药降糖制剂中非法掺入二甲双胍、苯乙双胍、格列吡嗪和格列本脲的有效检测方法。Objective：To develop a specific method for the identification of metformin,glyburide,glipizide and phenformin illegally added into Chinese medicine antidiabetic preparations.Methods：The liquid chromatography-ion trap mass spectrometry method was used.LC：Agilent C18 column（150 mm×4.6 mm,5 μm）,the mobile phase consisting of acetonitrile（phase A）,0.02 moL·L-1ammonium acetate（per 1000 mL contains 1.0 mL acetic acid,phase B）,and methanol（phase C）with gradient elution,a flow rate of 0.4 mL· min-1,column temperature 25 ℃.MS：positive electrospray ionization（ESI＋）and two scan modes including full scan MS and full scan MS-MS,the scanning range of 40-600 m/z,the drying gas temperature of 350 ℃,the drying gas flow rate of 10 L·min-1,the drying gas pressure of 276kPa,the ionization voltage of 5 kV.After separated by HPLC,the organic extraction of Chinese medicine preparations was analyzed.The obtained pseudo molecular ions,fragment ions and retention time were used to identify and determinate the four drugs by comparison with reference substances.Results：Three traditional Chinese medicine preparations were identified.One was mixed by Metformin and Glyburide,another was mixed by Phenformin and Glyburide and another was not found illegally mixed.Conclusion：The method is specific,sensitive accurate,thus may be used to detect the illegal traditional Chinese medicine antidiabetic preparations.

关 键 词：液相色谱—离子阱质谱联用 中药降糖制剂 二甲双胍 苯乙双胍 格列吡嗪 格列本脲 

分 类 号：R917[医药卫生—药物分析学]