固相萃取-高效液相色谱／串联质谱法同时测定牛奶中阿特拉津及其两类代谢物的残留

建立了高效液相色谱质谱联用检测牛奶中阿特拉津及其两类代谢物残留的同步分析方法。样品中加入1％HCl和0265mol／LNa2S2O3后，由冰乙腈提取，混合型阳离子交换柱固相萃取净化，采用液相色谱一串联质谱进行测定，外标法定量。阿特拉津及其代谢物在0．4～100μg几范围内线性良好，标准曲线相关系数R2〉0．99。在1～25μg／L浓度范围内，除脱异丙基羟基阿特拉津的平均加标回收率较低约为64．2％外，其它目标物的回收率在75．0％～119．0％之间，相对标准偏差为1．5％～14．5％；脱乙基阿特拉津、羟基阿特拉津、脱乙基羟基阿特拉津的检出限为0．1ug／L；其余目标物的检出限为0．5μg/L。...

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Bibliographic Details
Published in分析化学 Vol. 41; no. 1; pp. 128 - 132
Main Author 石冬冬 常碧影 刘庆生 石波
Format Journal Article
LanguageChinese
Published 中国农业科学院饲料研究所,北京,100081%中国农业科学院农业质量标准与检测技术研究所,北京,100081 2013
Subjects
代谢物
液相色谱质谱联用
牛奶
阿特拉津
阿特拉津
代谢物
牛奶
液相色谱质谱联用
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Summary:建立了高效液相色谱质谱联用检测牛奶中阿特拉津及其两类代谢物残留的同步分析方法。样品中加入1％HCl和0265mol／LNa2S2O3后，由冰乙腈提取，混合型阳离子交换柱固相萃取净化，采用液相色谱一串联质谱进行测定，外标法定量。阿特拉津及其代谢物在0．4～100μg几范围内线性良好，标准曲线相关系数R2〉0．99。在1～25μg／L浓度范围内，除脱异丙基羟基阿特拉津的平均加标回收率较低约为64．2％外，其它目标物的回收率在75．0％～119．0％之间，相对标准偏差为1．5％～14．5％；脱乙基阿特拉津、羟基阿特拉津、脱乙基羟基阿特拉津的检出限为0．1ug／L；其余目标物的检出限为0．5μg/L。本方法的灵敏度较高，且简便、快速，可以较好地解决目标物极性差别大及样品基质对检测结果的干扰等问题，可以满足牛奶中阿特拉津及其两类代谢物残留检测的需要。
Bibliography:Liquid chromatography-tandem mass spectrometry ; Milk ; Atrazine ; Metabolites
SHI Dong-Dong , CHANG Bi-Ying, LIU Qing-Sheng , SHI Bo （ Institute of Feed Research, Chinese Academy of Agricultural Sciences, Beijing 100081, China） 2 （ Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beifing 100081, China ）
22-1125/O6
A sensitive LC-MS method was developed for the determination of atrazine and its metabolites in cattle milk. The method can be applied to the simultaneous determination of atrazine and its major dealkylation and hydroxylation metabolites which include atrazine, hydroxyatrazine, diaminochloroatrazine, desisopropylatrazine, desethylatrazine, deethylhydroxyatrazine, deisopropylhydroxyatrazine. The analytical scheme including sample preparation, chromatographic and mass spectrometric conditions was developed and optimized. Hydrochloric acid and sodium thiosulphate were added to the sample before extracted by ice aeetonitrile. The mixed catio
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2013.20341