输港植物源性调味品中农药残留检测方法

The analysis method of pesticides residue in Hongkong plant-derived spices

目的针对2012年5月香港特区政府发布全新的食物中残余除害剂管理制度——《香港食物中残余除害剂的建议规管方案》(简称《规管方案》)中所涉及的共计7大类植物源性调味品中25项农药残留,建立相关样品处理及仪器测定方法。方法样品用含0.1%乙酸乙腈溶液超声提取,经SAX/PSA固相萃取柱净化,分别用气相色谱-质谱联用仪、气相色谱-串联质谱联用仪及液相色谱-串联质谱联用仪进行定性、定量分析。分别对蒜粉、姜粉及辣椒粉基质进行了50μg/kg水平上的添加回收实验,优化了前处理过程及仪器分析过程中几个关键步骤。结果检测结果添加回收率在67.8%~123.7%之间,确立了针对植物源性调味品中25项农药残留的分析和确认方法。结论该方法简单便捷,易于操作,有效地解决了植物源性调味品中复杂基质对测定农药残留的影响。

Objective To establish a method for the related samples’ pretreatment and instrument detection, regarding the 25 pesticide residues in the 7 major categories of plant derived spices which are involved in the new residual pesticides in food management system--“Hongkong foods recommended gauge residual pesticides tube scheme” (referred to as “regulatory scheme”) issued in 2012 May by the Hongkong SAR government.MethodsBy using acetonitrile with 0.1% acetic acid as the solvent, the sample was ultrasonic extracted, cleaned by SAX/PSA, and qualitatively and quantitatively analyzed by gas chromatography-mass (GC-MS), gas chromatography-mass/mass (GC-MS/MS) and liquid chromatography-mass/mass (LC-MS/ MS). In the experiment of recovery test on garlic powder, ginger powder and chilli powder spiked with 50 μg/kg, several key steps were optimized in the pretreatment process and instrument testing.Results The recoveries of those pesticides were from 67.8% and 123.7%. The analysis and confirmation method of plant source in the condiment of 25 pesticide residues were verified.ConclusionThis method is simple and easy to operate, and can effectively solve the impact of complex matrix in plant-derived spices on the detection of pesticide residues.