超高效液相色谱-四极杆-飞行时间质谱法快速筛查牛奶中的农药和兽药残留  

Determination of residues of pesticides and veterinary drugs in milk by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

作　　者：高馥蝶[1,2] 赵妍 邵兵[1,2] 张晶[1,2] 

机构地区：[1]首都医科大学公共卫生与家庭医学学院,北京100069 [2]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [3]南京市产品质量监督检验院,江苏南京210028

出　　处：《色谱》2012年第6期560-567,共8页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑计划项目(2011BAK10B06);北京市卫生局青年基金项目

摘　　要：利用超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)技术建立了牛奶中42种农药和兽药残留的快速检测方法。目标药物包括常用的13种农药和29种兽药,采用QuEChERS(Quick,Easy,Cheap,Effective,Rugged,and Safe)方法进行样品前处理。牛奶样品经含1%甲酸的乙腈溶液提取,同时加入无水硫酸钠和氯化钾盐析,提取液经C18填料净化后直接测定。目标药物经ACQUITY UPLCTMBEH C18柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,采用正离子全信息串联质谱扫描模式(MSE)进行检测。结果表明,牛奶中42种农药和兽药的定量限(LOQ,S/N=10)为1～100μg/kg;3个加标水平的平均回收率为68.2%～129.1%,相对标准偏差为2.8%～30.8%。该方法快速简便、灵敏度较高,可用于牛奶中42种农兽药的快速筛查。An analytical method was established for the simultaneous determination of 42 pesti- cides and veterinary drugs in milk by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry （UPLC-Q-TOF-MS）. The target compounds are the commonly used drugs including 13 pesticides and 29 veterinary drugs. The QuEChERS （ Quick, Easy, Cheap, Effective, Rugged, and Safe） method was used for sample preparation. The analytes in milk samples were extracted with acetonitrile containing I. 0% （v/v） formic acid, and were salted out by adding anhydrous sodium sulfate and potassium chloride. After that, the extract solution was purified by dispersive solid phase extraction with C l8 sorbent. In the chromatographic analysis of 42 target compounds were separated on an ACQUITY UPLCTM BEH C I8 column with the gradient elution using the mobile phases of acetonitrile and water containing 0. 1% formic acid. MSE （ where E represents collision energy） acquisition under posi- tive ion mode was performed to obtain accurate relative molecular masses and fragment ions. As a result, the limits of quantification （LOQ, S/N = 10） of the target compounds were from l ~g/kg to 100 ~g/kg in milk. The average recoveries of the 42 analytes spiked at three concen- tration levels were ranged from 68.2% to 129. 1% with the relative standard deviations of 2.8%- 30.8%. This method can be applied to the analysis of the 42 pesticides and veterinary drugs in milk due to its fastness, simplicity and relatively high sensitivity.

关 键 词：超高效液相色谱-四极杆-飞行时间质谱 QUECHERS 农药残留 兽药残留 牛奶 

分 类 号：O658[理学—分析化学]