基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留

doi:10.3724/SP.J.1123.2017.02032

色谱 ›› 2017, Vol. 35 ›› Issue (7): 719-723.DOI: 10.3724/SP.J.1123.2017.02032

基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留

秦美玲, 柴爽爽, 马有宁, 高欢欢, 张涵彤, 何巧

中国水稻研究所, 农业部稻米及制品质量监督检验测试中心, 农业部稻米产品质量安全风险评估实验室, 浙江杭州 310006

收稿日期:2017-02-27 出版日期:2017-07-08 发布日期:2013-10-18
通讯作者: 马有宁,Tel:(0571)63348941,E-mail:11116088@zju.edu.cn
基金资助:
国家农产品质量安全风险评估项目（GJFP2016001001）；中央级公益性科研院所基本科研业务费专项资金项目（2014RG006）.

Determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry based on QuEChERS

QIN Meiling, CHAI Shuangshuang, MA Youning, GAO Huanhuan, ZHANG Hantong, HE Qiao

Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Rice, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China

Received:2017-02-27 Online:2017-07-08 Published:2013-10-18
Supported by:
National Agricultural Product Quality Safety Risk Assessment Project (No.GJFP2016001001);Central Public Welfare Scientific Research Basic Business Expenses Special Funds for Scientific Research Projects (No.2014RG006).

摘要/Abstract

摘要：

采用改良的QuEChERS-液相色谱-串联质谱（LC-MS/MS）技术，建立了稻米中嘧草醚和双草醚残留量的检测方法。样品经酸化乙腈提取，由十八烷基键合硅胶（C₁₈）吸附剂净化。以0.1%（体积分数）甲酸水（含5 mmol/L乙酸铵）-乙腈为流动相进行梯度洗脱，经ZORBAX SB C₁₈色谱柱实现目标化合物的基线分离。采用电喷雾正离子（ESI⁺）模式扫描，动态多反应监测（dynamic MRM）技术定性分析，外标法定量。结果表明：在稻米基质中，嘧草醚和双草醚在各自的线性范围内线性关系良好（r²≥0.996）；嘧草醚和双草醚的检出限（LOD）分别为0.8和3 μ g/kg。在3个添加水平下，嘧草醚和双草醚的平均回收率分别为76.6%~85.6%和73.0%~86.7%，相对标准偏差（RSD）分别为0.9%~3.4%和1.2%~5.5%（n=6）。该方法简便、快速、灵敏，适用于稻米中嘧草醚和双草醚的同时分析。

关键词: QuEChERS, 稻米, 嘧草醚, 双草醚, 液相色谱-串联质谱

Abstract:

A method was developed for the determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with modified QuEChERS. The samples were extracted with acidified acetonitrile, and then purified by octadecylsilane bonded silica (C₁₈) adsorbents. The analytes were separated on a ZORBAX SB C₁₈ column through a gradient elution using 0.1% (v/v) aqueous formic acid aqueous containing 5 mmol/L ammonium acetate and acetonitrile as mobile phases. Positive electrospray ionization (ESI⁺) was used. Qualitative work was performed using selected dynamic multiple reaction monitoring (dynamic MRM) mode. Quantization was performed using external standard method. The results showed good linearities of pyriminobac-methyl and bispyribac-sodium with correlation coefficients (r²) not less than 0.996. The limits of detection (LODs) of the method were 0.8 μ g/kg for pyriminobac-methyl, and 3 μ g/kg for bispyribac-sodium. The mean spiked recoveries of pyriminobac-methyl and bispyribac-sodium at three spiked levels were 76.6%-85.6% and 73.0%-86.7%, respectively, and the relative standard deviations (RSDs) of pyriminobac-methyl and bispyribac-sodium were 0.9%-3.4% and 1.2%-5.5%, respectively. This method is simple, rapid, sensitive, and suitable for the simultaneous determination of pyriminobac-methyl and bispyribac-sodium in rice.

Key words: bispyribac-sodium, liquid chromatography-tandem mass spectrometry (LC-MS/MS), pyriminobac-methyl, QuEChERS, rice

中图分类号:

O658

秦美玲, 柴爽爽, 马有宁, 高欢欢, 张涵彤, 何巧. 基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留[J]. 色谱, 2017, 35(7): 719-723.

QIN Meiling, CHAI Shuangshuang, MA Youning, GAO Huanhuan, ZHANG Hantong, HE Qiao. Determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry based on QuEChERS[J]. Chinese Journal of Chromatography, 2017, 35(7): 719-723.

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基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留

Determination of pyriminobac-methyl and bispyribac-sodium residues in rice by liquid chromatography-tandem mass spectrometry based on QuEChERS

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