QuEChERS-气相色谱-质谱法测定土壤中6种酰胺类除草剂残留

发布时间：2018-04-02 07:43

本文选题：气相色谱-质谱　切入点：QuEChERS　出处：《色谱》2017年12期

【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0.999 6~1.000 0。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。
[Abstract]:A method was established for simultaneous determination of Acetochlor, alachlora, metolachloror, pyramidine, butachloror, butachloror and promethylamine in soil by QuEChERS- gas chromatography-mass spectrometry. Residues of amides in soil. 10 mL deionized water was extracted with 10 mL acetonitrile and 4 g NaCl. N- propyl ethylenediamine (PSAA) C18, graphitized carbon black (GCBB) and anhydrous magnesium sulfate (MgSO4) were purified and determined by gas chromatography-mass spectrometry. HP-5MS capillary column with weak polarity was used for gas chromatographic separation. In the mode of electron bombardment ionization ionization ionization (ei) source, the selective ion monitoring (SIM) scanning mode was used to detect the herbicides. The results showed that there was a good linear relationship between the six kinds of herbicides in the range of 0.01 ~ 1.00 mg/L. The correlation coefficient (r) is 0.999 ~ 1.0000.The average recovery rate of the six kinds of amide herbicides is 92.0 ~ 108.The relative standard deviation is 1.64 ~ 8.25g / kg, the detection limit is 0.0020.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg. The average recovery rate of six kinds of amide herbicides is 92.0 ~ 108g / kg. The detection limit is 0.0020.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg / g. The relative standard deviation is 1.64% ~ 8.25mg / kg. The detection limit of the method is 0.002 0.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg. Comparison of capture detection with GC-ECD, The method can improve the anti-interference ability and make 6 kinds of amide herbicides better separated. The method uses less organic solvents and amounts of organic solvents, and is easy to operate, fast, and has application value.
【作者单位】：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;
【基金】：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)~~
【分类号】：O657.63;X833

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