气质联机分析蔬菜中农药多残留及基质效应的补偿  

Rapid Determination of Pesticide Multiresidues in Vegetable by Gas Chromatography-mass Spectrometry and Compensation for Matrix Effect with Protectants

作　　者：黄宝勇[1] 潘灿平[1] 王一茹[2] 曹喆[2] 张微[1] 李文明[1] 江树人[1] 

机构地区：[1]中国农业大学理学院应用化学系 [2]安捷伦公司亚太区北京环境分析实验室,北京100083

出　　处：《高等学校化学学报》2006年第2期227-232,共6页Chemical Journal of Chinese Universities

基　　金：国家重点基础研究发展规划(批准号:2002CB410805)资助

摘　　要：建立了蔬菜中52种农药化合物的气相色谱一质谱检测方法，考察了基质效应和分析保护剂在方法中的应用，评价了3种分析保护剂组合的加入对补偿基质效应的影响，确定了最佳配比．样品前处理采用乙腈提取，用PSA（Primary—secondary amine）固相材料分散净化技术，用气质联机在选择离子监测模式下分析检测．该方法在0．01—1．00mg／L范围内线性关系良好，相关系数大于0．98，最低检测浓度除溴氰菊酯和异菌脲外均在0．2-9．4mg／kg之间，各化合物添加回收率为81．8％-119．5％，相对标准偏差为0．8％-17．6％．A multi-residue method is described for rapid determination of 52 multi-class pesticides, including their isomers, in vegetables by gas chromatography-mass spectrometry （GC-MS） with the aid of analyte proteetants. Addition of different combinations of proteetants before injection for compensation of matrix effect was demonstrated. Pesticides were extracted from samples with acetonitrile and the extract was cleaned up by using dispersive method by primary-secondary amine sorbent. Pesticides was injected into GC with the aid of analyte protectants [ 3-ethoxy-1,2-propanediol （ 20 mg/mL） and D-sorbitol （ 1 mg/mL） ] , followed by MS detection under El ionization and selective ion monitoring mode. Good linear and lower limits of detection were obtained, the linear range are between 0.01 and 1.00 mg/L, correlation coefficients are better than 0.98, and the detection limits are mainly between 0. 2 and 9. 4μg/kg. All compounds have mean recoveries of 81.8%-119.5% and the relative standard deviation is between 0.8% and 17.6%.

关 键 词：基质效应 农药多残留 气相色谱-质谱法 分析保护剂 

分 类 号：O657.63[理学—分析化学]