大豆中磺酰脲类除草剂残留量的检测
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R15 S565.1[著者标引]

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国家科技基础条件平台重点项目(2003DIA6N003)This work was supported by the National Science and Technology Program Funds of Ministry of Sdence and Technology China.


Multiresidue analysis of sulfonylurea herbicides in soybeans
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    摘要:

    为检测大豆中除草剂的残留量,建立了RP-HPLC和HPLC-MS选择离子监测(SIR)同时检测大豆中10种磺酰脲类除草剂残留量的方法。试样经乙腈提取,正己烷液-液分配,弗罗里硅土填充柱净化,然后采用RP-HPLC-DAD和HPLC-ESI(+)-MS测定。对HPLC和LC/MS分离条件、试样前处理条件进行了研究和优化。建立的方法简便、快速、灵敏。10种磺酰脲类除草剂HPLC法测定,在0.1-10.01μ/ml范围内线性相关系数为0.9996—0.9997,在0.05—2.00mg/kg浓度范围之间,加标回收率均在69.8%-100.7%,其多次测定的RSD在1.9%-10.4%之间,最低检出限均为20μg/kg。LC-MS法测定在0.025—1.0μg/ml范围内线性相关系数为0.9995—0.9998,在0.02-0.1mg/kg浓度范围之间,加标回收率均在72.1%-98.8%,其多次测定的RSD在0.9%-7.7%之间,最低检出限均低于10μg/kg。本方法可满足进、出口大豆中多种除草剂残留量同时检验的工作需要。

    Abstract:

    Reversed-phase high performance liquid chromatography and high performance liquid chromatography/electrospray ionization mass spectrometry have been developed for the simultaneous determination of multiple sulfonylurea herbicide residues in soybeans. Sulfonylurea herbicides were extracted from soybean samples with acetonitrile, and partitioned by hexane. After the extract was cleaned up with florisil column, sulfonylurea herbicides were analyzed by HPLC-DAD and HPLC-ESI(+)-MS and quantified by external standard method. Sample pre-treatment, LC and LC-MS analytical conditions were examined and optimized. The results indicated that the methods developed are easy, fast and sensitive. It also demonstrated that these multiresidue analysis methods can meet the requirements of simultaneous determination of multiple sulfonylurea herbicides for inspection of soybeans.

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祁彦 张新忠 杨强 储晓刚.大豆中磺酰脲类除草剂残留量的检测[J].中国食品卫生杂志,2005,(6).

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