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高效液相色谱法同时测定大豆中十种磺酰脲类除草剂残留量

[Simultaneous determination of ten sulfonylurea herbicide residues in soybeans by high performance liquid chromatography].

作者信息

Qi Yan, Zhan Chunrui, Zhang Xinzhong, Chu Xiaogang

机构信息

China Import & Export Commodity Inspection Technology Institute, Beijing 100025, China.

出版信息

Se Pu. 2004 Nov;22(6):634-8.

Abstract

A reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous determination of ten sulfonylurea herbicide (oxasulfuron, thifensulfuron-methyl, metsulfuron-methyl, triasulfuron, chlorsulfuron, bensulfuron-methyl, prosulfuron, pyrazosulfuron-methyl, chlorimuron-ethyl and primisufuron-methyl) residues in soybeans. Sulfonylurea herbicides were extracted with acetonitrile, followed by hexane partitioning. After the extract was cleaned up with a Florisil column, sulfonylurea herbicides were analyzed by HPLC-photo diode array detector (DAD) and quantified by external standard method. The pre-treatment method of the samples and the chromatographic conditions of the analysis were critically examined. The linear ranges of 10 sulfonylureas were 0.1 - 10.0 mg/L, and the correlation coefficients were 0.999 6 - 0.999 7. The average recoveries of ten sulfonylurea herbicides in spiked soybeans ranged from 69.8% to 100.7%, and the relative standard deviations were between 1.89% and 10.43%. The limit of detection was 20 microg/kg. The results have indicated that the method developed is easier, faster, and has better purification effect. It has also demonstrated that this multiresidue analytical method can meet the requirements for the simultaneous determination of many sulfonylurea herbicides in import and export inspection for soybeans.

摘要

建立了一种反相高效液相色谱(RP-HPLC)法,用于同时测定大豆中10种磺酰脲类除草剂(恶唑磺隆、噻吩磺隆、甲磺隆、醚苯磺隆、氯磺隆、苄嘧磺隆、丙苯磺隆、吡嘧磺隆、氯嘧磺隆和氟嘧磺隆)的残留量。磺酰脲类除草剂用乙腈提取,然后用正己烷分配。提取物经弗罗里硅土柱净化后,用高效液相色谱-光电二极管阵列检测器(DAD)分析,外标法定量。对样品的预处理方法和分析的色谱条件进行了严格考察。10种磺酰脲类除草剂的线性范围为0.1 - 10.0 mg/L,相关系数为0.999 6 - 0.999 7。加标大豆中10种磺酰脲类除草剂的平均回收率为69.8%至100.7%,相对标准偏差在1.89%至10.43%之间。检测限为20 μg/kg。结果表明,所建立的方法更简便、快速,净化效果更好。还表明,这种多残留分析方法能够满足进出口大豆检验中多种磺酰脲类除草剂同时测定的要求。

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