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固相萃取-高效液相色谱/质谱串联法分析奶牛饮用水中莠去津及其6种代谢物的残留
引用本文:石冬冬,常碧影,石波,田园.固相萃取-高效液相色谱/质谱串联法分析奶牛饮用水中莠去津及其6种代谢物的残留[J].中国农业科技导报,2012,14(6):145-152.
作者姓名:石冬冬  常碧影  石波  田园
作者单位:(1.中国农业科学院饲料研究所, 北京 100081,2.中国农业科学院农业质量标准与检测技术研究所, 北京 100081)
基金项目:中央级公益性科研院所基本科研业务费专项(1610332012013)资助
摘    要:建立了高效液相色谱质谱联用检测奶牛饮用水中莠去津及其6种代谢物残留的同步分析方法。利用MCX固相萃取柱富集净化,采用液相色谱-质谱串联进行测定,外标法定量。结果表明莠去津及其代谢物在0.4~100 μg/L范围内线性良好,标准曲线相关系数r2均大于0.99。在0.03~3 μg/L浓度范围内,平均加标回收率除脱异丙基羟基莠去津的较低(64.17%)外,其他目标物的回收率在71.31%~116.67%之间,相对标准偏差为0.97%~12.03%。7种目标物的检出限为0.01 μg/L,方法的灵敏度较高,且简便、快速。

关 键 词:莠去津  液相色谱质谱联用  饮用水  代谢物  

Determination of Trace Atrazine and its Six Metabolites in Water by Solid Phase Extraction and Liquid Chromatography/Mass Spectrometry
SHI Dong-dong,CHANG Bi-ying,SHI Bo,TIAN Yuan.Determination of Trace Atrazine and its Six Metabolites in Water by Solid Phase Extraction and Liquid Chromatography/Mass Spectrometry[J].Journal of Agricultural Science and Technology,2012,14(6):145-152.
Authors:SHI Dong-dong  CHANG Bi-ying  SHI Bo  TIAN Yuan
Institution:(1.Institute of Feed Research, Chinese Academy of Agricultural Sciences, Beijing 100081|2.Institute of Quality Standard and Testing Technology for Agro Products, CAAS, Beijing 100081, China)
Abstract:A sensitive LC MS/MS method for simultaneously analyzing atrazine and its 6 metabolites in cattle drinking water was established. The samples were enriched and purified by MCX solid phase column, determined by LC MS/MS, and quantified by outer standard. The results showed that the linear range spanned from 0.4 to 100 μg/L with correlation index r2 greated than 0.99. At the concentration range of 0.03~3 μg/L, except the recovery of desisopropyl 2 hydroxy was 6417%, others were 71.31%~116.67% with relative standard deviations ranging from 097% to 12.03%. The limits of detection (LOD) of 7 substances analyses were 0.1 μg/L. Those indicated the method was rapid, cost effective and suitable for water sample analysis.
Keywords:atrazine  HPLC MS  drinking water  metabolites  
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