QuECHERS前处理法测定生鲜乳中六种氨基甲酸酯农药残留  

Determination of six carbamate pesticide residues in raw milk by QuECHERS pretreatment

作　　者：黄波[1] Huang Bo(Fujian Agricultural Product Quality and Safety Inspection and Testing Center,Fuzhou,350003)

机构地区：[1]福建省农产品质量安全检验检测中心,福州350003

出　　处：《福建畜牧兽医》2022年第5期20-22,共3页Fujian Journal of Animal Husbandry and Veterinary medicine

摘　　要：建立生鲜乳中涕灭威、涕灭威砜、涕灭威亚砜、甲萘威、霜霉威和灭多威六种氨基甲酸酯农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法,样品经乙腈提取后,加入氯化钠振摇、离心后取上清液加入QuECHERS净化包(内含PSA、GCB、C18、MgSO4)净化后经超高效液相色谱-串联质谱仪和C18色谱柱分离,以甲醇、甲酸-乙酸铵水溶液为流动相梯度洗脱。电喷雾离子源正离子扫描,多反应离子监测检测,对检测样品进行外标法定量。数据表明:六种氨基甲酸酯农药标准溶液在10~100μg/kg添加水平的回收率为78.67%~104.12%,该方法具有操作简单、花费时间少、灵敏度比较高、定性和定量都比较准确等优点,可用于生鲜乳中部分氨基甲酸酯类农药的检测。An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of six carbamate pesticide residues, including aldicarb, aldicarb sulfone, aldicar sulfoxide, carbaryl, propamocarb and methomyl in raw milk. The sample was extracted with acetonitrile, added with sodium chloride, shaken and centrifuged, and the supernatant was added into a QuECHERS purification package(containing PSA, GCB, C18 and MgSO4) for purification, and then separated by ultra performance liquid chromatography-tandem mass spectrometer and C18 chromatographic column with methanol and formic acid-ammonium acetate aqueous solution as mobile phase for gradient elution. Lectrospray ion source positive ion scan, multiple reaction ion monitoring detection, and external standard method quantification of that detect sample. The results showed that the recoveries of six carbamate pesticides were 78.67% ~104.12% in the range of 10 ~100 μg/kg.The method was simple, sensitive, accurate and could be used for the determination of some carbamate pesticides in raw milk.

关 键 词：QUECHERS 生鲜乳 氨基甲酸酯 农药 残留 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]