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
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0.4~100μg/L范围内线性良好,标准曲线相关系数r2均大于0.99。在0.03~3μg/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0.01μg/L,方法的灵敏度较高,且简便、快速。...
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Published in | 中国农业科技导报 Vol. 14; no. 6; pp. 145 - 152 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
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
2012
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Subjects | |
Online Access | Get full text |
ISSN | 1008-0864 |
DOI | 10.3969/j.issn.1008-0864.2012.06.23 |
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Summary: | 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0.4~100μg/L范围内线性良好,标准曲线相关系数r2均大于0.99。在0.03~3μg/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0.01μg/L,方法的灵敏度较高,且简便、快速。 |
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Bibliography: | 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 des isopropyl-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. SHI Dong-dong, CHANG Bi-ying, SHI Bo , TIAN Yuan 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 11-3900/S atrazine ; HPLC-MS ; drinking water; met |
ISSN: | 1008-0864 |
DOI: | 10.3969/j.issn.1008-0864.2012.06.23 |