液相色谱-串联质谱法测定枸杞中氨基甲酸酯类农药残留量  

Determination of 8 Carbamate Pesticide Residues in Lycium by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张艳[1] 王晓菁[1] 

机构地区：[1]农业部枸杞产品质量监督检验测试中心,宁夏银川750002

出　　处：《河南农业科学》2011年第2期107-110,共4页Journal of Henan Agricultural Sciences

基　　金：国家科技支撑计划(2009BAI72B00)

摘　　要：建立了同时测定枸杞中涕灭威亚砜、涕灭威砜、灭多威、3-羟基克百威、涕灭威、克百威、抗蚜威、甲萘威8种氨基甲酸酯类农药残留的液相色谱-串联质谱(LC-MS/MS)检测方法。枸杞样品经乙腈提取,Carbon/NH2小柱净化,C18柱分离后,在电喷雾正离子化模式下,于三重四极杆质谱仪上以多反应监测方式测定。结果表明:8种农药在20～500μg/L之间线性关系良好,且r≥0.99;8种农药的方法检出限(S/N=3)为0.01～5μg/kg。对枸杞样品分别进行0.02、0.05、0.1 mg/kg 3个水平的加标回收试验,其平均回收率分别为77.7%～98.6%、85.0%～103.8%和76.8%～102.2%;相对标准偏差分别为2.48%～9.98%、4.14%～10.40%和8.33%～18.80%。该方法快速、准确、灵敏,适合对枸杞中涕灭威亚砜等8种氨基甲酸酯类农药残留的同时分析。A liquid chromatography-tandem mass spectrometric（LC-MS/MS）method was developed for simultaneous determination of aldicarb-sulfoxide,aldicarb-sulfone,methomyl,carbofuran-3-hydroxy,aldicarb,carbofuran,pirimicarb and carbaryl carbamates pesticides in Lycium.The sample was extracted with acetonitrile,and then cleaned up by Carbon/NH2 cartridge.8 pesticides were separated on a C18 column using 2 mmol/L ammonium acetate（A）-acetonitrile（B） as mobile phase in gradient elution.The analytes were detected with positive-ion electrospray ionization-mass spectrometry in MRM mode.Under the optimal conditions,the calibration curve was linear in the range of 20-500 μg/L and the detection limit（S/N=3）ranged from 0.01 to 5 μg/kg.The results showed that the mean recoveries of 8 pesticides at three spiked concentration levels of 0.02,0.05 and 0.1 mg/kg were in the range of 77.7%-98.6%,85.0%-103.8% and 76.8%-102.2%,respectively,with relative standard deviations（RSDs） of 2.48%-9.98%,4.14%-10.40% and 8.33%-18.80%,respectively.The method is rapid,sensitive and reliable,suitable for analyzing carbamate pesticide residues in Lycium.

关 键 词：液相色谱-串联质谱 农药残留 枸杞 

分 类 号：O657.63[理学—分析化学]