中文摘要：本文构建了一种经济快速的多残留检测方法，该方法采用QuEChERS技术联合DLLME萃取技术进行样本预处理，然后采用GC-MS技术定量检测不同果蔬中36种农药残留（13种有机氯、11种有机磷和12种拟除虫菊酯）。实验结果发现：本文采用QuEChERS和DLLME萃取方法，省略了PSA 清洗步骤，其检测结果与原来使用PSA 清洗结果类似，而且精度在12%以内，检测限在0.001-0.010μg/kg之间，0.05mg/kg加标水平下的回收率在87%-106%之间。应用该方法对印度勒克瑙市的果蔬样本中三种农药（高效氯氰菊酯、高效氯氟氰菊酯、毒死蜱）残留进行检测分析，结果显示农药残留量高于MRL值。与昂贵的PSA 清洗步骤相比，使用基于QuEChERS和DLLME萃取联用的GC-MS技术检测方法，不仅经济快速，而且不影响检测的精准度，因此广泛适用于多种果蔬农药的常规检测。
外文摘要：An economical and rapid multiresidue method has been developed using quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure combined with dispersive liquid-liquid microextraction (DLLME) for the quantitative determination of 36 multiclass, multiresidue pesticides (13 organochlorines, 11 organophosphates, and 12 synthetic pyrethroids) in different vegetables and fruits without primary and secondary amine (PSA) cleanup step followed by gas chromatography-mass spectrometry (GC-MS) analysis. The procedure mainly involves the acetonitrile extraction in the presence of anhydrous MgSO4 and NaCl followed by DLLME using carbon tetrachloride (extraction solvent) and acetonitrile (disperser solvent). Experimental parameters were optimized using design of experiments (DoE) approach. The method developed without PSA cleanup step has yield similar analytical performance with that of method with PSA cleanup step for all the pesticides analyzed. The precision of the developed method was found to be less than 12 % and limit of detection for all the analyzed pesticides was found to be in the range of 0.001-0.010 mg kg(-1). This method was successfully applied in different fruits and vegetables and the recoveries were found to be in the range of 87-106 % at 0.05 mg kg(-1) with an acceptable precision (< 16 %). Coupling of QuEChERS with DLLME may be an appropriate replacement to eliminate costly PSA and makes the QuEChERS method more economical, time saving, without losing its analytical efficiency. The samples collected from Lucknow City, India, were analyzed for the presence of pesticides and only three pesticides beta-cypermethrin, lambda-cyhalothrin, and chlorpyrifos were found to have value above PFA-1954/CODEX-MRL values. The method has immense utility to use it for routine analysis of multiclass, multiresidue pesticides in fruits and vegetables.
外文关键词：Multiclass-multiresidue analysis；QuEChERS；Dispersive liquid-liquid microextraction (DLLME)；Primary secondary amine (PSA)
作者：Rai, Satyajeet；Singh, Abhishek Kumar；Srivastava, Anshuman
作者单位：Pesticide Toxicology Laboratory, Regulatory Toxicology Group,CSIR-Indian Institute of Toxicology Research (CSIR-IITR), MG Marg, Lucknow, Uttar Pradesh 226001, India
期刊名称：Food Analytical Methods
期刊影响因子：2.167
出版年份：2016
出版刊次：2
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