摘要
研究了选择离子气相色谱-质谱法测定乳及乳制品中2,6-二异丙基萘、七氟菊酯等17种拟除虫菊酯类农药残留的方法,优化了预处理方法和气相色谱-质谱分析条件。乳制品以乙腈为提取溶剂,采用匀浆提取,经C18及氟罗里硅土固相萃取小柱净化,采用气相色谱-质谱法测定和确证,选择离子监测模式,外标法定量。结果表明,17种农药在0.01~1.00 mg/L范围内呈线性关系,在0.01~0.2 mg/kg范围内的加标回收率为76%~114%,相对标准偏差为7.0%~16.2%,检出限为0.002~0.010 mg/kg,定量下限为0.010~0.030 mg/kg,方法能满足国内外乳制品中菊酯类农药残留限量水平的要求。
A gas chromatography-mass spectrometric method was developed for the determination of 17 pyrethroid pesticides residues,such as 2,6-diisopropylnaphtalene,tefluthrin,etc,in dairy under selected ion monitoring（SIM） mode.According to the chemical properties of samples,the pretreatments of the method and the mass spectrometric parameters were optimized.The liquid samples were salted-out directly with sodium chloride（NaCl）.The solid samples were soaked with water,and then salted-out with NaCl.The samples were extracted using acetonitrile by homogenate extraction technology and cleaned up by C18 column and Florisil solid-phase extraction.The analytes were confirmed and determined by GC-MS under selected ion monitoring mode.The calibration curves of 17 pyrethroid pesticides were linear in the range of 0.01-1.00 mg/L.The recoveries at spiked concentrations of 0.01-0.2 mg/kg ranged from 76% to 114% with relative standard deviations（RSDs） of 7.0%-16.2%.The detection limits and quantitation limits of 17 pyrethroid pesticides were in the range of 0.002-0.010 mg/kg and 0.010-0.030 mg/kg,respectively.The method could meet the requirements for the maximum residue levels（MRLs） of pyrethroid pesticides established by the European Union（EU） and China.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第9期948-952,共5页
Journal of Instrumental Analysis
基金
国家质检总局科研课题资助项目(2009IK164)
