湖北农业科学 ›› 2019, Vol. 58 ›› Issue (1): 96-99.doi: 10.14088/j.cnki.issn0439-8114.2019.01.023

• 检测分析 • 上一篇    下一篇

QuEChERS-气相色谱串联质谱法检测诺丽酵素原液中12种农药残留

吴南村1, 2, 张群1, 2, 刘春华1, 2, 马晨1, 2, 吴学进1, 2   

  1. 1.中国热带农业科学院分析测试中心,海口 571101;
    2.海南省热带果蔬产品质量安全重点实验室,海口 571101
  • 收稿日期:2018-06-13 出版日期:2019-01-10 发布日期:2019-11-26
  • 作者简介:吴南村(1982-),女,海南海口人,助理研究员,硕士,主要从事农产品农药残留分析研究,(电话)0898-66895007(电子信箱)nancy3412@163.com。

Simultaneous Determination of Fermentation Broth of Morinda Citrifolia using QuEChERS-Gas Chromatography-tandem Mass Spectrometry

WU Nan-cun1, 2, ZHANG Qun1, 2, LIU Chun-hua1, 2, MA Chen1, 2, WU Xue-jin1, 2   

  1. 1. Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China;
    2.Hainan Key Laboratory for Quality and Safety of Tropical Fruits and Vegetables,Haikou 571101,China
  • Received:2018-06-13 Online:2019-01-10 Published:2019-11-26

摘要: 建立了QuEChERS净化结合气相色谱串联质谱测定诺丽酵素原液中12种农药残留的方法。样品采用乙腈溶液提取,提取液中加入无水硫酸镁、氯化钠、柠檬酸钠、柠檬酸氢二钠脱水和缓冲,振荡分层后吸取上层清液,再经PSA净化离心后上机。结果表明,50 mg PSA能够满足方法的净化要求,12种农药均采用外标法定量,基质标准溶液在0.005~0.960 mg/L线性良好;在0.012、0.080、0.400 mg/kg 3个添加水平下回收率为84.2%~113.0%,RSD均小于15%,大部分农药定量限为0.012 mg/kg。该方法前处理简单快速,准确度和精密度符合检测要求,可满足诺丽酵素原液中的乙烯菌核利、腐霉利、联苯菊酯等12种农药残留的同时检测。

关键词: 诺丽酵素原液, 农药, QuEChERS, 气相色谱串联质谱

Abstract: A method has been developed for the simultaneous determination of 12 pesticides residues in fermentation broth of Morinda citrifolia using QuEChERS-gas chromatography-tandem mass spectrometry. The residue of 12 pesticides were extracted from samples by acetonitrile,then the extracting solution was cleaned up with PSA. Finally,the pesticides was analysed by gas chromatography-mass spectrometry under MRM mode via electrospray ionization.All pesticides were quantified by external standard method. The matrix calibration curves of the pesticides were linear in the range of 0.005~0.960 mg/L. The average recoveries of target compounds at three spiked concentration levels of 0.012,0.08,0.40 mg/kg were in the range of 84.2%~113.0%, RSD were less than 15%, the limit of quantification of most pesticides were 0.012 mg/kg. The results demonstrated the method is simple, fast aaccurated and can be used for analysis of the multiclass of pesticide residues in fermentation broth of morinda citrifolia.

Key words: Morinda citrifolia, pesticides, QuEChERS, gas chromatography-tandem mass spectrometry

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