食品科学 ›› 2010, Vol. 31 ›› Issue (16 ): 217-219.doi: 10.7506/spkx1002-6630-201016047

• 分析检测 • 上一篇    下一篇

气相色谱- 质谱法测定粮谷中5 种除草剂残留

屠海云,姜 荷,李 玮*   

  1. 杭州市质量技术监督检测院
  • 收稿日期:2010-04-20 出版日期:2010-08-25 发布日期:2010-12-29
  • 通讯作者: 李 玮* E-mail:liw@hzzjy.net

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

TU Hai-yun,JIANG He,LI Wei *   

  1. (Hangzhou Institute of Test and Calibration for Quality and Technology Supervision, Hangzhou 310019, China)
  • Received:2010-04-20 Online:2010-08-25 Published:2010-12-29
  • Contact: LI Wei * E-mail:liw@hzzjy.net

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。

关键词: 乙二胺氮丙基硅烷, 气相色谱- 质谱, 除草剂, 粮谷

Abstract:

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 acetonitrile 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 performed 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.

Key words: primary secondary amine (PSA), gas chromatography-mass spectrometry (GC-MS), herbicide, cereals

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