快速滤过型净化法结合高效液相色谱-串联质谱同时检测人参中的5种农药残留

基于人参样品基质特点，采用快速滤过型净化法 (m-PFC) 结合高效液相色谱-串联质谱 (HPLC-MS/MS)，建立了人参中嘧菌酯、苯醚甲环唑、吡虫啉、茚虫威和噻嗪酮5种农药残留同时检测的分析方法。该方法具有较低的检出限 (0.03~0.18 μg/kg) 和定量限 (0.11~0.59 μg/kg)，其定量限较中国国家标准GB 2763—2016中规定的对人参中苯醚甲环唑和嘧菌酯的最大残留限量 (MRL) (0.5~1 mg/kg) 低3个数量级，5种农药的线性范围在1~500 μg/L之间。在2、10、50、100和300 μg/kg的添加水平下，方法的平均回收率均在76%~115%之间，相对标准偏差 (RSD) 均小于11%，回收率较好且方法稳定。与传统样品前处理方法相比，该方法具有操作简单、省时省力和灵敏度高等优点。将该方法应用于市售6份人参样品中5种农药残留的检测，结果未检出相应的农药残留。该方法为研发建立更快速、准确地检测人参中农药残留的方法提供了思路，也为后续中国国家标准修订人参中农药最大残留限量提供了参考。

Simultaneous detection of five pesticide residues in ginseng by multi-plug filtration cleanup method combined with high performance liquid chromatography-tandem mass spectrometry

Based on the characteristics of ginseng samples matrix, a method for simultaneous determination of azoxystrobin, difenoconazole, imidacloprid, indoxacarb and thiazinone residues in ginseng was established by multi-plug filtration cleanup (m-PFC) method combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A low detection limits (LOD, 0.03-0.18 μg/kg) and quantitative limits (LOQ, 0.11-0.59 μg/kg) were obtained. The LOQ is three orders lower than the limit for azoxystrobin (1 mg/kg) and difenoconazole (0.5 mg/kg) in ginseng in GB 2763—2016. The linear range for five pesticides can reach to 1-500 μg/L. The average recovery rate of the method was between 76% and 115%, with RSD less than 11% at the spiking levels of 2, 10, 50, 100 and 300 μg/kg. Compared with the traditional sample pretreatment method, the new method has the advantages of simple operation, time-saving, labor-saving, and high sensitivity. The method was successfully applied to the detection of five pesticides in six ginseng samples. No corresponding pesticide residues were detected. This method provides a direction for rapid and accurate detection of pesticide residues in ginseng. It also provides a reference for revising the maximum residue limits of pesticides in ginseng in the national standard.