QuEChERS-SPE结合超高效液相色谱-四级杆飞行时间质谱法筛查牛奶样品中15类37种药物残留  

Simultaneous Determination for 15 Kinds of 37 Drugs in Milk Using a QuEChERS-SPE-based Method and Ultra Performance Liquid Chromatography Coupled with Quadrupole-time of Flight Mass Spectrometry

作　　者：李永利[1] 陈黎明[1] 李杰[1] 李春华[1] 陈鹰[1] LI Yong-li;CHEN Liming;LI Jie;LI Chun-hua;CHEN Ying(Shanghai Institute of Measurement and Testing Technology,Shanghai 201203,China)

机构地区：[1]上海市计量测试技术研究院,上海201203

出　　处：《化学试剂》2020年第4期406-410,共5页Chemical Reagents

基　　金：上海市科学技术委员会科研计划项目(17142203200)。

摘　　要：采用QuEChERS-SPE结合超高效液相色谱-飞行时间质谱(UPLC-Q-TOF-MS)技术开发了快速测定牛奶中15类37种药物的方法。牛奶样品采用0.2%甲酸乙腈溶液和Na2EDTA-Mcllvaine缓冲溶液提取,有机相和水相分别经C18吸附剂和HLB固相萃取柱净化后合并测定。目标化合物采用BEH C18柱分离,以甲醇和0.1%甲酸水溶液为洗脱剂进行程序洗脱,正离子扫描模式检测。结果表明,牛奶样品中化合物的定量限为0.4~8.0μg/kg,3个加标浓度的平均回收率范围为70.2%~105.3%。方法具有快速、简便、高通量等特点,可以用于牛奶样品15类37种药物残留的快速测定。A method was developed for rapid identification of 37 drugs in milk based on QuEChERS-SPE by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS).The target analysts in milk were extracted with acetonitrile containing 0.2%formic acid.The organic phase was purified with dispersive solid phase extraction with C18 sorbent,while the aqueous phase was cleaned with solid phase extraction.The target compounds were separated on a BEH C18 column with the gradient elution using the mobile phases of methanol and water containing 0.1%formic acid.The accurate relative molecular masses were obtained under positive ion mode.As a result,the limits of quantification(LOQ,S/N=10)of the compounds were from 0.4 to 8.0μg/kg in milk.Based on blank sample,the average recoveries of the 37 compounds set at three concentration levels were ranged from 70.2%to 105.3%.The method can be applied to the determination of the 15 kinds of 37 drugs in milk by virtue of its fastness,simplicity,and high-throughput.

关 键 词：液相色谱-四级杆飞行时间质谱 QUECHERS 药物残留 筛查 牛奶 

分 类 号：O657.6[理学—分析化学]