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食品研究与开发:2016,37(7):128-132
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分散固相萃取-液质联用法检测玉米中4种农药
赵风年,石梦琪,李辉,邵华,张超,李腾飞,刘广洋,王珊珊,王静*,金茂俊,金芬,郑鹭飞,佘永新*
(中国农业科学院 农业质量标准与检测技术研究所/农业部农产品质量安全重点实验室,北京 100081)
Determination of 4 Pesticides in Corns by Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction
ZHAO Feng-nian, SHI Meng-qi, LI Hui , SHAO Hua, ZHANG Chao, LI Teng-fei, LIU Guang-yang , WANG Shan-shan ,WANG Jing*, JIN Mao-jun, JIN Fen, ZHENG Lu-fei, SHE Yong-xin*
(Key Lab of Agro-product Quality and Safety of Chinese Agricultural Ministry, Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081,China)
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投稿时间:2016-01-10    
中文摘要: 利用分散固相萃取(QuEChERS)改良技术建立了玉米中多菌灵、吡虫啉、乙草胺、异丙甲草胺残留的液相色谱串联质谱分析方法。样品经 1 %甲酸乙腈提取,采用 N-丙基乙二胺(PSA)和十八烷基键合硅胶(C18)共萃取净化, C18 色 谱柱分离, 0.1 %甲酸-乙腈为流动相梯度洗脱,质谱采用电喷雾正离子(ESI+)模式电离,多离子检测模式(MRM)定性, 基质标准曲线外标法进行定量分析。结果表明:玉米基质中多菌灵、吡虫啉、乙草胺、异丙甲草胺在 0.5 μg/kg~100 μg/kg 浓度 范围内,具有很好的线性关系,其相关系数(R)均大于 0.995。在 3 个加标浓度下,4 种农药的平均回收率在 88.0 %~ 112.0 %之间,相对标准偏差(RSD, n=5)不大于 9.5 %。该方法对多菌灵、吡虫啉、乙草胺和异丙甲草胺的检出限分别为0.025、0.15、0.15 μg/kg 和 0.025 μg/kg,满足玉米中 4 种农药残留分析的要求。
Abstract:A simple pesticide analysis method was developed for the determination of carbendazim, imidaclo- prid, acetochlor and metolachlor in corns based on dispersive solid phase extraction procedure combined with liquid chromatography-positive mode electrospray ionization-tandem mass spectrometric (LC-MS/MS). The analytes were extracted with acid acetonitrile and cleaned up by primary secondary amine(PSA) and octadecyl silane (C18). Qualitative and quantitative analyses were carried out for four analytes under the positive scanning models after the chromatographic separation on reversed phase C18 column with an gradient elution program of acetonitrile and 0.1 % formic acid aqueous solution. The coefficient of determination(R) was > 0.995 within the calibration linearity range of 0.5 μg/kg-100 μg/kg for the four peaticides. The average recoveries of carbendaz- im, imidacloprid, acetochlor and metolachlor in corn samples were in the range 88.0 %-112.0 %with associat- ed RSDs (n=5)≤ 9.5 % at the three spiked level. The limits of detection (LOD)of four analytes were 0.025,0.15, 0.15 μg/kg and 0.025 μg/kg, respectively. The method could meet the determination requirements of these four pesticides in corns.
文章编号:201607031     中图分类号:    文献标志码:A
基金项目:公益性行业(农业)科研专项(201203094)
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