黄芪中氟啶虫酰胺和除虫菊素残留量及膳食风险评估

Residues and Dietary Risk Assessments of Flonicamid and Pyrethrin in Astragalus membranaceus

[目的]采用超高效液相色谱-串联质谱技术建立黄芪中氟啶虫酰胺和除虫菊素含量的快速检测方法,明确氟啶虫酰胺和除虫菊素在黄芪中的最终残留量,并进行膳食风险评估,为其在黄芪上的安全合理使用提供依据。[方法]样品经乙腈提取,MgSO4、PSA和GCB净化管净化后,超高效液相色谱-串联质谱(UPLC-MS/MS)检测。[结果]氟啶虫酰胺、除虫菊素I和除虫菊素II在质量浓度为0.002~0.10 mg/L的基质标准溶液中线性关系良好,相关系数R2均在0.999以上,在黄芪中的定量限均为0.01 mg/kg。在0.01、0.10、0.20 mg/kg添加水平下,氟啶虫酰胺、除虫菊素I和除虫菊素II的平均回收率为80.07%~105.69%,相对标准偏差为1.01%~13.06%。根据最终残留数据,计算氟啶虫酰胺和除虫菊素的国家估算每日摄入量(NEDI)为0.0015 mg,风险商值(RQ)分别为0.32‰和0.57‰。[结论]该方法操作简便且灵敏度高,适用于供试2种杀虫剂的残留检测。氟啶虫酰胺和除虫菊素在施药剂量分别为66.67、8.33 g/hm2时,不会对一般人群健康造成不可接受的风险。

[Aims] This study aims to develop a rapid method for the determination of flonicamid and pyrethrin in Astragalus membranaceus by ultra performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS). To provide evidence for their safe and rational use, the terminal residues and dietary risk assessment of flonicamid and pyrethrin were evaluated in Astragalus membranaceus. [Methods] The samples were extracted with acetonitrile, purified by Mg SO4, PSA and GCB purification tubes, and detected by UPLC-MS/MS. [Results] The linearities of flonicamid, pyrethrin I and pyrethrin II were satisfied with correlation coefficents of above 0.999 in the range of 0.002-0.10 mg/L. The mean recoveries ranged from 80.07 to 105.69% with the relative standard deviations(RSDs) of 1.01-13.06% at fortification levels of 0.01, 0.10 and 0.20 mg/kg. The limits of quantification(LOQs) were both 0.01 mg/kg. Based on the terminal residue data, the national estimated daily intakes(NEDIs) of flonicamid and pyrethrin in general population were both 0.0015 mg, and the risk quotient was 0.32 and 0.57‰, respectively.[Conclusions] The simple and sensitive method was suitable for the determination of flonicamid and pyrethrin residues in A. membranaceus. Fluticamid and pyrethrin might not cause unacceptable risk to the health of the general population at the dosage of 66.67 and 8.33 g/ha, respectively.