色谱 ›› 2017, Vol. 35 ›› Issue (12): 1317-1321.DOI: 10.3724/SP.J.1123.2017.09003

• 研究论文 • 上一篇    

QuEChERS-气相色谱-质谱法测定土壤中6种酰胺类除草剂残留

梅文泉, 黎其万, 方海仙, 耿慧春, 陈兴连   

  1. 云南省农业科学院质量标准与检测技术研究所, 农业部农产品质量监督检验测试中心, 云南 昆明 650223
  • 收稿日期:2017-09-02 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 梅文泉,Tel:(0871)65140430,E-mail:wenquan_mei@hotmail.com
  • 基金资助:

    云南省科技创新平台建设计划项目(2014DA001);云南省创新团队计划项目(2015HC025).

Determination of six amide herbicide residues in soil by QuEChERS-gas chromatography-mass spectrometry

MEI Wenquan, LI Qiwan, FANG Haixian, GENG Huichun, CHEN Xinglian   

  1. Agri-Food Quality Standard and Testing Technology Institute, Yunnan Academy of Agricultural Science, Supervision & Testing Center for Farm Products Quality Ministry of Agriculture, Kunming Section, Kunming 650223, China
  • Received:2017-09-02 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Science and Technology Innovation Platform Construction Project of Yunnan Province (No. 2014DA001); Innovative Team Plan Project of Yunnan Province (No. 2015HC025).

摘要:

建立了QuEChERS-气相色谱-质谱同时测定土壤中乙草胺(acetochlor)、甲草胺(alachlor)、异丙甲草胺(metolachlor)、吡草胺(metazachlor)、丁草胺(butachlor)和丙草胺(pretilachlor)6种酰胺类除草剂的分析方法。土壤中残留的酰胺类除草剂用10 mL去离子水、10 mL乙腈和4 g NaCl提取,用N-丙基乙二胺(PSA)、C18、石墨化炭黑(GCB)和无水硫酸镁(MgSO4)净化,然后用气相色谱-质谱联用法测定。采用HP-5MS弱极性石英毛细管柱进行气相色谱分离,在电子轰击电离(EI)源模式下以选择离子监测(SIM)扫描模式检测。结果表明,6种酰胺类除草剂在0.01~1.00 mg/L范围内呈良好线性关系,相关系数(r)为0.9996~1.0000。在加标水平为0.025、0.10和0.50 mg/kg时,6种酰胺类除草剂的平均回收率为92.0%~108%,相对标准偏差为1.64%~8.25%(n=3)。方法的检出限为0.002~0.006 mg/kg,定量限为0.005~0.02 mg/kg。同常用的气相色谱-电子捕获检测(GC-ECD)法比较,该法可提高抗干扰能力,使6种酰胺类除草剂得到较好分离。方法所使用的有机溶剂种类和用量少,操作简单、快速,具有应用价值。

关键词: QuEChERS, 残留, 气相色谱-质谱, 土壤, 酰胺类除草剂

Abstract:

A method was developed for the determination of six amide herbicides, such as acetochlor, alachlor, metolachlor, metazachlor, butachlor and pretilachlor, by QuEChERS-gas chromatography-mass spectrometry. The soil samples were extracted by 10 mL acetonitrile, 10 mL deionized water and 4 g sodium chloride, then purified with 50 mg N-propyl ethylenediamine (PSA), 50 mg C18, 10 mg graphitized carbon black (GCB) and 100 mg MgSO4. Low-polar silica capillary column HP-5MS was used. The extracts were detected by electron impact ionization (EI) source in the selected ion monitoring (SIM) mode. The results showed that good linearities were obtained with the mass concentrations of the six amide herbicides in the range of 0.01-1.00 mg/L, and their correlation coefficients ranged from 0.9996 to 1.0000. Under the condition of adding contents of 0.025, 0.10 and 0.50 mg/kg, the average recoveries of the six amide herbicides ranged from 92.0% to 108%, and the relative standard deviations were 1.64%-8.25%. The limits of detection (LODs) were 0.002-0.006 mg/kg and the limits of quantification (LOQs) were 0.005-0.02 mg/kg. Comparing with the gas chromatography-electron capture detection (GC-ECD) which used to detect the amide herbicides, this method can improve the anti-interference ability, and get better separation of the six amide herbicides. The method has the advantages of simplicity, rapidity, and application value.

Key words: amide herbicides, gas chromatography-mass spectrometry (GC-MS), QuEChERS, residues, soil

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