色谱 ›› 2018, Vol. 36 ›› Issue (11): 1173-1180.DOI: 10.3724/SP.J.1123.2018.06015

• 研究论文 • 上一篇    下一篇

QuEChERS-气相色谱-质谱联用法快速测定人参中农药多残留

崔丽丽, 闫梅霞, 朴向民, 逄世峰, 王英平   

  1. 中国农业科学院特产研究所, 吉林 长春 130112
  • 收稿日期:2018-06-20 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 王英平.Tel:(0431)81919806,E-mail:yingpingw@126.com.
  • 基金资助:

    中国农业科学院科技创新工程项目(CAAS-ASTIP-2016-ISAPS);吉林省科技发展计划项目(20170309007YY,20170623038TC).

Rapid determination of pesticide multiresidues in panax ginseng by QuEChERS-gas chromatography-mass spectrometry

CUI Lili, YAN Meixia, PIAO Xiangmin, PANG Shifeng, WANG Yingping   

  1. Institute of Special Wild Economic Animals and Plants, Chinese Academy of Agricultural Sciences, Changchun 130112, China
  • Received:2018-06-20 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    Science and Technology Innovation Project of Chinese Academy of Agricultural Sciences (No. CAAS-ASTIP-2016-ISAPS); Jilin Province Science and Technology Development Plan Project (Nos. 20170309007YY, 20170623038TC).

摘要:

建立了QuEChERS-气相色谱-质谱联用(GC-MS)法同时测定人参中20种农药残留量的检测技术。样品前处理采用改进的QuEChERS方法,人参粉加水浸润后,用乙腈均质提取,用N-丙基乙二胺(PSA)和MgSO4净化,结合GC-MS检测系统,在电子轰击源(EI)选择离子监测(SIM)模式下进行检测,使用HP-5毛细管柱进行分离。在优化条件下,20种农药在一定范围内线性关系良好,相关系数大于0.990,方法检出限(信噪比S/N=3)为0.001~0.007 mg/kg,定量限(S/N=10)为0.002~0.024 mg/kg,平均回收率为70.41%~114.06%,相对标准偏差(RSD)为0.76%~15.47%。该方法操作简单快捷、灵敏度高。

关键词: QuEChERS, 农药, 气相色谱-质谱, 人参

Abstract:

In this study, the extraction and purification improvements of the QuEChERS method were coupled with gas chromatography-mass spectrometry (GC-MS) to determine 20 pesticides in panax ginseng. Dry ginseng powder was mixed with water, and the solution was then extracted with acetonitrile and purified with N-propylethylenediamine (PSA) and MgSO4 to remove co-extractives that might interfere with the results. The target compounds were detected after electron-impact ionization in selected ion monitoring (SIM) mode. Under optimum conditions, the method gave a good linear relationship for the determination of the pesticides within a certain concentration range, with correlation coefficients greater than 0.990. Moreover, the limits of detection (S/N=3) were 0.002-0.007 mg/kg, the limits of quantification (S/N=10) were 0.002-0.024 mg/kg, and the average recoveries for pesticides in panax ginseng were 70.41%-114.06%, with relative standard deviations of 0.76%-15.47%. In comparison with previous methods, the new procedure has the advantages of simple sample preparation and higher sensitivity.

Key words: panax ginseng, gas chromatography-mass spectrometry (GC-MS), pesticides, QuEChERS

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