色谱

色谱 ›› 2016, Vol. 34 ›› Issue (2): 158-164.DOI: 10.3724/SP.J.1123.2015.09026

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留

张爱芝1, 王全林1, 曹丽丽1, 李誉1, 沈昊1, 沈坚1, 张书芬1, 满正印1,2   

  1. 1. 宁波市产品质量监督检验研究院, 浙江 宁波 315048;
    2. 宁波大学海洋学院, 浙江 宁波 315211
  • 收稿日期:2015-09-23 出版日期:2016-02-08 发布日期:2012-09-11
  • 通讯作者: 王全林
  • 基金资助:

    宁波市科技服务业示范项目(2013F10019).

Determination of 250 pesticide residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

ZHANG Aizhi1, WANG Quanlin1, CAO Lili1, LI Yu1, SHEN Hao1, SHEN Jian1, ZHANG Shufen1, MAN Zhengyin1,2   

  1. 1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315048, China;
    2. School of Marine Sciences, Ningbo University, Ningbo 315211, China
  • Received:2015-09-23 Online:2016-02-08 Published:2012-09-11
  • Supported by:

    Ningbo Science and Technology Service Demonstration Project (2013F10019).

PDF

317

被引次数

49

摘要：

以QuEChERS为前处理方法,超高效液相色谱-串联质谱为检测仪器,建立了蔬菜中250种农药残留的快速筛查检测方法。采用含1%(v/v)乙酸的乙腈溶液提取样品,以无水硫酸镁(MgSO4)作为脱水剂,经MgSO4、丙基乙二胺(PSA)、石墨化碳(GCB)、C18混合净化剂净化,Waters ACQUITYTM UPLC BEH C18柱(100 mm×2.1 mm, 1.7 μ m)分离,超高效液相色谱-串联质谱进行测定。实验详细考察了MgSO4、PSA、GCB、C18用量对农药添加回收率的影响,结果表明,2 mL提取上清液中加入300 mg MgSO4、200 mg PSA、10 mg GCB和100 mg C18时净化效果最好。250种农药在韭菜中3个添加水平下的回收率为60.1%~120.0%,相对标准偏差(RSD)为3.5%~19.5%;检出限为0.01~50.00 μ g/kg。该方法简便、快速、可靠,可用于蔬菜中多种农药残留的快速筛查与确证的日常工作中,具有一定的推广价值。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 农药多残留, 蔬菜

Abstract:

A multiresidue analytical method for the determination of 250 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with acetonitrile containing 1%(v/v) acetic acid, purified by a mixed sorbent of MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and C18, separated on a Waters ACQUITYTM UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μ m) and detected by UPLC-MS/MS. Anhydrous magnesium sulfate was used as a dewatering agent. The effects of the amounts of MgSO4, PSA, GCB and C18 added on the recoveries of 250 pesticides were investigated. The results showed that the purification effect was best when 300 mg MgSO4, 200 mg PSA, 10 mg GCB and 100 mg C18 in 2 mL of the extract were added. For the 250 pesticide residues, the limits of detection (LODs) of the method were from 0.01 to 50.00 μ g/kg. The recoveries obtained ranged from 60.1% to 120% at three spiked levels in Chinese chives with the relative standard deviations between 3.5% and 19.5% using matrix matched external standard method. The results showed that the method is able to meet requirements of the multiresidue detection of the 250 pesticides in vegetable. The method has the advantages of rapidity, simplicity, high sensitivity and better purification effect. It is suitable for the rapid determination of the common pesticides in vegetables, and it provides a strong guarantee for the risk assessments of the quality and safety of vegetables.

Key words: pesticide multiresidues, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), vegetables

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