食品科学 ›› 2019, Vol. 40 ›› Issue (12): 326-331.doi: 10.7506/spkx1002-6630-20180411-139

• 安全检测 • 上一篇    下一篇

灵芝中17 种农药的QuEChERS-气相色谱-质谱联用快速检测技术

崔丽丽,闫梅霞,逄世峰,周春元,王英平*   

  1. 中国农业科学院特产研究所,吉林 长春 130112
  • 出版日期:2019-06-25 发布日期:2019-06-28
  • 基金资助:
    中国农业科学院科技创新工程项目(CAAS-ASTIP-2016-ISAPS);吉林省省级医药健康产业发展专项(20180311021YY)

Simultaneous Determination of Seventeen Pesticide Residues in Ganoderma tsugae by Modified QuEChERS Combined with Gas Chromatography-Mass Spectrometry

CUI Lili, YAN Meixia, PANG Shifeng, ZHOU Chunyuan, WANG Yingping*   

  1. Institute of Special Wild Economic Animals and Plants, Chinese Academy of Agricultural Sciences, Changchun 130112, China
  • Online:2019-06-25 Published:2019-06-28

摘要: 建立改进的QuEChERS提取和净化方法,结合气相色谱-质谱联用法测定灵芝中17 种农药残留的检测方法。干燥的灵芝粉加水浸润后,经乙腈均质提取,正丙基乙二胺、MgSO4净化去杂,结合气相色谱-质谱检测系统,电子电离源,HP-5毛细管柱分离,程序升温,离子扫描模式检测。在优化条件下17 种杀菌剂在一定质量浓度范围内线性关系良好,相关系数大于0.98,方法检出限(RSN=3)在0.002~0.022 mg/kg之间,定量限(RSN=10)在0.007~0.072 mg/kg之间,方法的平均回收率为71.10%~119.55%,相对标准偏差为0.47%~20.05%。本方法具有操作简单快捷、灵敏度高等优点。

关键词: QuEChERS, 气相色谱-质谱联用法, 灵芝, 农药

Abstract: In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample pretreatment method coupled with gas chromatography-mass spectrometry (GC-MS) was established to determine 17 pesticide residues in Ganoderma tsugae. A total of 1.0 g of dry G. tsugae powder was mixed with 10 mL of water, and then extracted by homogenization with aceonitrile. The extract was cleaned up with n-propyl ethylenediamine (PSA) and MgSO4 to remove the interferences from co-extractives. The separation was accomplished on an HP-5 capillary column and programmed heating was carried out. The target compounds were detected by electron impact ionization in the single ion monitoring (SIM) mode. Under the optimum conditions, the method showed a good linear relationship for all these pesticides in certain concentration ranges, with correlation coefficients greater than 0.98. Moreover, the limits of detection (LODs) (RSN = 3) were 0.002–0.022 mg/kg, the limits of quantitation (LOQs) (RSN =10) were 0.007–0.072 mg/kg. The average recoveries of this method were in the range of 71.10%–119.55% with relative standard deviations (RSDs) between 0.47% and 20.05%. In comparison with previous methods, the new procedure has the characteristics of simple sample preparation and higher sensitivity.

Key words: QuEChERS, gas chromatography-mass spectrometry, Ganoderma tsugae, pesticides

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