人参中吡唑醚菌酯和氟唑菌酰胺的残留分析及膳食风险评估

目的]建立人参中吡唑醚菌酯和氟唑菌酰胺的残留分析方法,分析2种农药在人参中的残留消解及最终残留量,评价其在人参上的安全性。方法]样品中的吡唑醚菌酯和氟唑菌酰胺用乙腈提取,PSA、C18和GCB净化,高效液相色谱-串联质谱法检测。结果]吡唑醚菌酯和氟唑菌酰胺在鲜人参、人参干粉和植株中的平均回收率在76.7%~105.3%和75.0%~98.6%之间,变异系数在1.5%~4.5%和0.8%~6.6%之间,最小检出量为1.86×10^-4、3.87×10^-4 ng。吡唑醚菌酯和氟唑菌酰胺在人参植株中的半衰期分别为0.2~8.4、19.7~21.8 d,在鲜人参中的最终残留量分别为0.010~0.139、0.010~0.248 mg/kg,在人参干粉中的最终残留量分别为0.010~0.203、0.011~0.535 mg/kg。吡唑醚菌酯和氟唑菌酰胺在鲜人参中的估计慢性膳食风险商分别为7.62×10^-3和1.28×10^-2,在人参干粉中的估计慢性膳食风险商分别为4.65×10^-3和7.30×10^-3,均小于1。结论]按照推荐施药方法,吡唑醚菌酯和氟唑菌酰胺在人参中的慢性膳食风险为可接受水平,建议我国2种农药在人参上的MRL值分别为0.5、2 mg/kg。

Residue Analysis and Dietary Risk Assessment of Pyraclostrobin and Fluxapyroxad in Ginseng

Aims]This study aims to establish a residual analytical method of pyraclostrobin and fluxapyroxad in Panax ginseng,the safety in P.ginseng was evaluated by analysis of residual dissipation and terminal residues.Methods]The residues of pyraclostrobin and fluxapyroxad in the three sample matrixes were extracted with acetonitrile and the extracts were purified by PSA,C18 and GCB,the residue amount was detected by HPLC-MS/MS.Results]The average fortified recoveries of pyraclostrobin and fluxapyroxad in three sample matrixes(fresh ginseng,ginseng dry powder and plants)were respectively between 76.7-105.3 and 75.0-98.6%with the relative standard deviations of 1.5-4.5 and 0.8-6.6%,and the limit of detection was 1.86×10^-4 and 3.87×10^-4 ng to two target analyses in three sample matrixes.The half-lives of pyraclostrobin and fluxapyroxad in ginseng plants were calculated by their first-order kinetics,the values were 0.2-8.4 and 19.7-21.8 d,respectively.And the terminal residual amounts of pyraclostrobin and fluxapyroxad were 0.010-0.139 and 0.010-0.248 mg/kg in fresh ginseng,and 0.010-0.203 and 0.011-0.535 mg/kg in ginseng dry powder,respectively.The chronic risk quotient of pyraclostrobin and fluxapyroxad in fresh ginseng were 7.62×10^-3 and 1.28×10^-2,and 4.65×10^-3 and 7.30×10^-3 in ginseng dry powder respectively.Conclusions]According to the recommended application method in the specifications,the chronic risk quotient of pyraclostrobin and fluxapyroxad in ginseng was acceptable.And the proposed MRL of pyraclostrobin and fluxapyroxad in ginseng were 0.5 and 2 mg/kg in China,respectively.