大豆中磺酰脲类除草剂残留量的检测  

Multiresidue analysis of sulfonylurea herbicides in soybeans

作　　者：祁彦[1] 张新忠[2] 杨强[1] 储晓刚[1] 

机构地区：[1]中国检验检疫科学研究院,北京100025 [2]中国农业大学理学院,北京100094

出　　处：《中国食品卫生杂志》2005年第6期501-504,共4页Chinese Journal of Food Hygiene

基　　金：国家科技基础条件平台重点项目(2003DIA6N003)~~

摘　　要：为检测大豆中除草剂的残留量,建立了RPHPLC和HPLCMS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RPHPLCDAD和HPLCESI(+)MS测定。对HPLC和LCMS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0.1～10.0μgml范围内线性相关系数为0.9996～0.9997,在0.05～2.00mgkg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20μgkg。LCMS法测定在0.025～1.0μgml范围内线性相关系数为0.9995～0.9998,在0.02～0.1mgkg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10μgkg。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。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 muhiresidue analysis methods can meet the requirements of simultaneous determination of multiple sulfonylurea herbicides for inspection of soybeans.

关 键 词：大豆 农药残留量 色谱法 高压液相 光谱分析 质谱 

分 类 号：R155.5[医药卫生—营养与食品卫生学]