›› 2012, Vol. 14 ›› Issue (6): 145-152.DOI: doi:10.3969/j.issn.10080864.2012.06.23

• 方法与技术创新 • 上一篇    

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

石冬冬1,常碧影2,石波1*,田园1   

  1. (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)
  • 出版日期:2012-12-15 发布日期:2012-12-17

Determination of Trace Atrazine and its Six Metabolites in Water by Solid Phase Extraction and Liquid Chromatography/
Mass Spectrometry

SHI Dong-dong1, CHANG Bi-ying2, SHI Bo1*, TIAN Yuan1   

  1. (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)
  • Online:2012-12-15 Published:2012-12-17

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

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.

Key words: atrazine, HPLCMS, drinking water, metabolites

中图分类号: