UPLC-MS/MS法测定中成药及保健品中添加的16种降糖类化学药物  

Determination of 16 anti-diabetic chemicals added to traditional Chinese medicines and health care products by UPLC-MS /MS

作　　者：屠婕红[1] 盛静[1] 丁宝月[1] 徐宏祥 傅应华[1] 

机构地区：[1]嘉兴学院医学院,嘉兴314001 [2]嘉兴市食品药品检验所,嘉兴314000

出　　处：《药物分析杂志》2014年第10期1823-1829,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：浙江省公益性技术应用研究计划资助项目(No.2013C37103);‘十二五’浙江省高校重点学科(药理学)资助项目

摘　　要：目的:建立快速、准确检测中成药及保健品中非法添加的16种降糖类化学药物的方法。方法:采用UPLC-MS/MS法,使用Waters Acquity BEH-C18(1.7μm,2.1 mm×50 mm),以0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱(0~3 min,32%A→50%A;3~6 min,50%A→60%A;6~9 min,60%A→70%A;9~11 min,70%A→90%A;11~12 min,90%A→90%A;12~13 min,90%A→32%A);流速:0.2 mL·min-1;柱温:40℃;选择ESI离子源、正离子扫描、多反应离子监测(MRM)模式测定16种降糖类化学药物。通过比较MRM通道中样品峰与对照品峰的分子离子峰,二级碎片离子峰、色谱保留时间等信息确定添加的化学药物,并根据外标法以质谱峰面积计算添加药物的准确量。结果:在上述色谱及质谱条件下,二甲双胍、丁二胍、苯乙双胍、罗格列酮、小檗碱、吡格列酮、氯磺丙脲、甲苯磺丁脲、妥拉磺脲、格列吡嗪、格列齐特、瑞格列奈、格列苯脲、格列美脲、那格列奈、格列喹酮等16种药物的分离度良好,方法定量下限(LOQ)均在0.2~1.5 ng·mL-1之间,标准加样回收率均在88.6%~116.9%之间。结论:本法快速准确,灵敏度高,可作为中成药及保健品中非法添加降糖类化学药物的定量测定方法。Objective ： To establish a rapid, accurate method for determination of 16 anti - diabetic chemicals, which were illegally added to traditional Chinese medicines and health care products. Methods： The UPLC - MS/MS method was adopted. The analytes were separated on a Waters Acquity BEH C^8 column （1.7 μm,2.1 mm × 50 mm） with 0.1% formic acid methanol （A） and 0.1% formic acid solution （B） as the mobile phase by gradient elution （0 -3 min,32% A→50% A;3 -6 min,50% A→60% A;6 - 9 min,60% A→70% A;9 - 11 min,70% A→90 % A ; 11 - 12 min, 90 % A→90 % A ; 12 - 13 min, 90 % A→32 % A） at a flow rate of 0.2 mL · min - 1, and the col- umn temperature was 40 ℃. A positive - ion （ ESI ＋ ） source and a MRM mode was used to separate and quantita- tively determinate 16 anti -diabetic chemicals. The obtained molecular ions, fragment ions and retention time for MRM channels were used to identify the 16 kinds of drugs by comparison with those of reference substances. The obtained peak areas were used to determinate the accurate content of anti - diabetic drugs in traditional Chinese medicines and health care products according to the external standard method. Results： A good resolution of 16 kinds of chemical drugs, including metformin, butylbiguanide, phenformin, rosiglitazone, berberine, pioglitazone, chlorpropamide, tolbutamide, tolazamide, glipizide, glielazide, repaglinide, geliebenniao, geliemeiniao, nateglinide and gliquidone was obtained under this UPLC and MS/MS condition. The limits of quantitation （LOQ） were in the range of 0.2 - 1.5 ng · mL- 1 and the standard addition recoveries were in the range of 88.6% - 116.9%. Conclusion ： The method is rapid, accurate and highly sensitive, which can be used for the determination of ille- gal added anti -diabetic chemicals in traditional Chinese medicines and health care products.

关 键 词：二甲双胍 丁二胍 苯乙双胍 罗格列酮 小檗碱 吡格列酮 氯磺丙脲 甲苯磺丁脲 妥拉磺脲 格列吡嗪 格列齐特 瑞格列奈 格列苯脲 格列美脲 那格列奈 格列喹酮 

分 类 号：R917[医药卫生—药物分析学]