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通过式固相萃取净化/超高效液相色谱-串联质谱法测定黄瓜、番茄及豇豆中的克百威与涕灭威残留
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覃国新,劳水兵,莫仁甫,闫飞燕,王静,金茂俊,何洁,周其峰,杨玉霞,王海军,陈伟 1.广西壮族自治区农业科学院农产品质量安全与检测技术研究所,农业部甘蔗品质监督检验测试中心(南宁)2.中国农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全重点实验室 
基金项目:广西省自然科学基金面上项目(2017GXNSFAA198231);广西省自然科学基金青年基金项目(2016GXNSFBA380147);广西科技重大专项(桂科AA17204043-2);广西农业科学院基本科研业务专项(2017YZ04,桂农科2018YT34);广西农业科学院科技发展基金项目(桂农科2018JZ09,桂农科2018JZ10,桂农科2018JZ11)
中文摘要:建立了黄瓜、番茄和豇豆中克百威和涕灭威及其代谢物3 羟基克百威、涕灭威砜、涕灭威亚砜的超高效液相色谱-串联质谱检测方法。样品经乙腈和QuEChERS(0.5 g柠檬酸二钠盐水合物、1 g 无水柠檬酸钠、1 g氯化钠、4 g MgSO4)提取盐包提取,Oasis PRiME HLB固相萃取柱通过式净化,超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测,采用空白基质匹配的校准曲线外标法定量。结果显示,2种农药及其代谢物均在0.001~0.5 mg/L范围内呈良好的线性关系,相关系数均大于0.996 0。在0.02~0.2 mg/kg加标浓度范围内的平均回收率为80.4%~110%,相对标准偏差(RSD)为1.1%~4.8%。克百威、3-羟基克百威、涕灭威、涕灭威砜和涕灭威亚砜的检出限(LOD)分别为0.07、0.3、1.0、4.0、13 μg/kg,定量下限(LOQ)分别为0.2、1.0、2.0、13、42 μg/kg。
中文关键词:通过式固相萃取  超高效液相色谱-串联质谱  黄瓜  番茄  豇豆  克百威  涕灭威  代谢物
 
Determination of Carbofuran and Aldicarb Residues in Cucumber,Tomato and Cowpea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of carbofuran and aldicarb,as well as their metabolites carbofuran 3-hydroxy,aldicarb sulfone and aldicarb sulfoxide in cucumber,tomato and cowpea.The samples were extracted with acetonitrile and QuEChERS salt packets containing 0.5 g sodium sesquihydrate,1 g sodium citrate,1 g NaCl and 4 g MgSO4,and purified by pass through solid phase extraction using an Oasis PRiME HLB column,then analyzed by UPLC-MS/MS.The matrix effects were observed in the analysis of the analytes in sample.The quantitations were performed by the external standard method with matrix matched calibration standards.There were linear relationships for carbofuran,carbofuran 3 hydroxy,aldicarb,aldicarb sulfone and aldicarb sulfoxide in the range of 0.001-0.5 mg/L with their correlation coefficients(r) larger than 0.996 0.Recoveries for cucumber,tomato and cowpea at spiked levels of 0.02-0.2 mg/kg ranged from 80.4% to 110%,with relative standard deviations(RSDs) of 1.1%-4.8%.The limits of detection(LOD,S/N=3) for carbofuran,carbofuran 3-hydroxy,aldicarb,aldicarb sulfone and aldicarb sulfoxide were 0.07,0.3,1.0,4.0 and 13 μg/kg,respectively,and the limits of quantitation(LOQ,S/N=10) were 0.2,1.0,2.0,13 and 42 μg/kg,respectively
Key Words:pass through solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  cucumber  tomato  cowpea  carbofuran  aldicarb  metabolites
引用本文:覃国新,劳水兵,莫仁甫,闫飞燕,王静,金茂俊,何洁,周其峰,杨玉霞,王海军,陈伟.通过式固相萃取净化/超高效液相色谱-串联质谱法测定黄瓜、番茄及豇豆中的克百威与涕灭威残留[J].分析测试学报,2019,(8):967-972.
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