气相色谱-质谱法测定粮谷中5种除草剂残留  

Determination of Five Herbicide Residues in Cereals by Gas Chromatography-Mass Spectrometry

作　　者：屠海云 姜荷[1] 李玮[1] 

机构地区：[1]杭州市质量技术监督检测院,浙江杭州310019

出　　处：《食品科学》2010年第16期217-219,共3页Food Science

摘　　要：建立气相色谱-质谱(GC-MS)法测定粮谷中残留的5种除草剂的方法。样品采用乙腈提取,乙二胺氮丙基硅烷(PSA)和氨基填料作为吸附剂净化,然后采用气相色谱-质谱测定,全扫描和选择离子监测模式同时检测,内标法单离子定量。结果表明:方法在0.05～0.5mg/L范围内呈现良好的线性关系,相关系数均大于0.999;在0.05、0.10、0.20mg/kg添加水平下,加标回收率在85%～99%之间,相对标准偏差(RSD)小于5%。采用基质分散固相萃取技术,实现样品的快速制备,有效地消除基质带来的干扰,灵敏度高,完全适合样品中5种除草剂残留量的日常批量检测和确证。A method was established for the determination of 5 herbicide residues （metolachlor, clomazone, acetochlor, metalaxyl and pyrazosulfuron） in cereals using gas chromatography-mass spectrometry （GC-MS）. Samples were extracted with acetoni-trile and cleaned up with primary secondary amine （PSA） and amino group packing materials. The analysis was carried out using GC-MS with electron impact （EI） source in a simultaneous full scan-selected ion monitoring mode. Quantification was per-formed using the internal standard method. This method exhibited good linearity within the range from 0.05 to 0.5 mg/L with a correlation coefficient of 0.999. Average recoveries for metolachlor in 6 cereal species spiked at 0.05, 0.1 mg/kg and 0.2 mg/kg ranged from 85% to 99%, with a RSD of smaller than 5%. For this method, matrix solid phase dispersion extraction used gives a rapid sample preparation approach. This method is free of interference from matrices and highly sensitive, and is exactly suitable for the daily large-scale determination of metolachlor, clomazone, acetochlor, metalaxyl and pyrazosulfuron residues in cereals.

关 键 词：乙二胺氮丙基硅烷 气相色谱-质谱 除草剂 粮谷 

分 类 号：TS207.7[轻工技术与工程—食品科学]