液相色谱-串联质谱测定降血糖功能食品中双胍类药物  

Determination of biguanides in antidiabetic functional foods by LC-MS/MS

作　　者：王雅[1] 郗存显[2] 向露[1] 王俊苏[2] 陈冬东[3] 彭涛[3] 王国民[2] 母昭德[1] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆出入境检验检疫局,重庆市进出口食品安全工程技术研究中心,重庆400020 [3]中国检验检疫科学研究院,北京100123

出　　处：《分析试验室》2013年第8期1-6,共6页Chinese Journal of Analysis Laboratory

基　　金："十二五"农村领域国家科技计划课题(2012BAD33B02);质检公益性行业科研专项(201010073);重庆市科委项目(CSTC2009CB1012)资助

摘　　要：建立了降血糖功能食品中二甲双胍和苯乙双胍的液相色谱-串联质谱测定方法。采用体积比1:1的甲醇-乙醇溶液超声提取降血糖功能食品降糖粉、奶粉、口服液、胶囊、清渴茶中的二甲双胍和苯乙双胍,提取液经WCX固相萃取柱净化后,以乙腈和2 mmol/L NH4Ac溶液(含0.1%甲酸)为流动相进行梯度洗脱,经Agilent ZORBAX Eclipse XDB-C18色谱柱分离,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质回收标准曲线定量。二甲双胍和苯乙双胍的定量限(LOQ)均为10.0μg/kg,在不同基质中添加水平为10.0,20.0,50.0μg/kg时,二甲双胍和苯乙双胍的平均回收率分别为92.7%～99.6%和91.3%～100.3%,RSD分别为2.1%～8.4%和1.1%～11%。本方法可用于降血糖功能食品中双胍类药物的测定和确证。A comprehensive analytical method based on liquid chromatography-tandem mass spectrometry（LCMS/MS） was developed for the determination of metformin and phenformin in antidiabetic functional foods.Samples including anti-diabetic powder,milk powder,oral liquid,capsule and diabetes tea were extracted ultrasonically with methanol-ethanol（50： 50,V/V）,cleaned up with WCX solid-phase extraction cartridges.The separation was performed on a Agilent ZORBAX Eclipse XDB-C18 column using the mobile phase composed of acetonitrile and 2 mmol/L ammonium acetate aqueous solution（containing 0.1% formic acid） with a gradient elution program.Tandem mass spectrometric detection was performed in multiple reaction monitoring（MRM） scan mode with a positive electrospray ionization（ESI＋） source.Quantification was done by the external matrixmatched standard curve.Both the limits of quantification（LOQ） of metformin and phenformin were 10.0 μg/kg.At spiking levels of 10.0,20.0 and 50.0 μg/kg in different matrices,average recoveries of metformin and phenformin were 92.7% ～ 99.6% and 91.3% ～ 100.3%,and RSD were 2.1% ～ 8.4% and 1.1% ～ 10.3%,respectively.The method developed was simple,reliable and sensitive,which can be used to determine and identify the biguanides in antidiabetic functional foods.

关 键 词：二甲双胍 苯乙双胍 功能食品 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]