色谱

色谱

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溶剂转移-气相色谱-质谱法和选择洗脱-气相色谱法测定大蒜中289种农药多残留

苏建峰1*, 卢声宇2, 陈晶1, 陈劲星1, 梁震1,2, 刘建军1,3   

  1. 1. 福建华日食品安全检测有限公司, 福建 福州 350015; 2. 福建出入境检验检疫局, 福建 福州 350001; 3. 中国检验认证集团福建有限公司, 福建 福州 350001
  • 收稿日期:2011-04-14 修回日期:2011-05-09 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 苏建峰,硕士,工程师,研究方向为食品中污染物残留分析. Tel: (0591)38132966
  • 基金资助:

    福建出入境检验检疫局科技计划项目(FK2008-14).

Multi-residue determination of 289 pesticides in garlic by gas chromatography and gas chromatography/mass spectrometry

SU Jianfeng1*, LU Shengyu2, CHEN Jing1, CHEN Jinxing1, LIANG Zhen1,2, LIU Jianjun1,3   

  1. 1. Fujian Fairreach Food Safety Testing Co., Ltd., Fuzhou 350015, China; 2. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China; 3. Fujian Co., Ltd. of China Certification & Inspection Group, Fuzhou 350001, China
  • Received:2011-04-14 Revised:2011-05-09 Online:2011-07-28 Published:2011-08-19

PDF

806

被引次数

53

摘要： 以溶剂转移净化为核心步骤,建立了一种适用于大蒜样品中农药多残留分析的前处理方法(方法I),配以一个辅助方法(方法II),构成大蒜中常见289种农药多残留的分析体系(方法I283种,方法II6种)。方法I中,样品用乙腈-水溶液提取,盐析分配,溶剂转移和固相萃取(SPE)净化后进行气相色谱-质谱(GC-MS)分析;方法II中,样品用无水Na2SO4配合乙酸乙酯均质研磨,超声波辅助提取,提取液经Primary Secondary Amine (PSA)粉末分散固相萃取和LC-Si柱选择洗脱净化后进行GC分析。GC-MS采用选择离子监测(SIM)方式,GC采用火焰光度检测器(FPD)检测,外标法定量。方法简便、快速,通过优化前处理和上机条件,在最优条件下进行测试,方法的定量限(S/N≥10)为0.01～0.05 mg/kg。方法I中,在加标水平为0.02、0.20 mg/kg时,回收率为52%～163%,其中回收率在70%～120%之间的占88%,相对标准偏差为2.4%～18%;方法II中,在加标水平为0.01、0.02、0.10、0.20 mg/kg时,回收率为70%～111%,相对标准偏差为3.2%～9.3%。详细描述了实验模型的构建,并对GC-MS灵敏度的提高提出了新的见解。该方法准确、灵敏、快速,可满足大蒜中多种农药残留的检测要求。

关键词: 大蒜, 多残留分析, 灵敏度, 农药, 气相色谱法, 气相色谱-质谱法, 样品前处理

Abstract: A new idea of solvent transfer technique was developed and applied to determine 283 pesticide residues in garlic by gas chromatography-mass spectrometry (GC-MS) (method I), and the other method using normal phase silica/selective elution technique was applied to determine 6 pesticide residues with strongly polar in garlic by gas chromatography (method II). For the method I, the residues were extracted from homogenized tissue with acetonitrile-water, separated with liquid-liquid partition; the clear supernatant was purified by solvent transfer technique and solid phase extraction (Envi-18 and LC-NH2 columns), then was analyzed by GC-MS. For the method II, the residues were extracted from homogenized tissue using ethyl acetate and sodium sulfate assisted by ultrasonication. The supernatant was purified by solid phase extraction (primary secondary amine (PSA) powder and LC-Si column) prior to GC analysis. The determination was performed by using selected ion monitoring (SIM) mode in GC-MS method and flame photometric detector (FPD) in GC method, then external standard method was used in the quantification. Under the optimal conditions, the detection limits for the two methods (S/N≥10) of pesticides were 0.01~0.05 mg/kg, the recoveries carried out by the addition of standards of 0.01~0.20 mg/kg were 52%~163%, among which the recoveries for 88% pesticides were between 70% and 120%; the recoveries of the method II were 70%~111%; while the relative standard deviations were 2.4%~18% and 3.2%~9.3%, respectively. The model of solvent transfer technique and the sensitivity improvement of GC-MS was also studied. The methods are easy, fast, more sensitive, and can meet the requirement of the multiresidual analysis in garlic.

Key words: garlic, gas chromatography-mass spectrometry (GC-MS), multiresidual analysis, pesticides, sample pretreatment, gas chromatography (GC), sensitivity