三七药材中262种农药多残留筛查及风险评估

目的:对三七中农药多残留进行筛查研究,初步了解其农药残留状况,并评估高检出农药的健康风险,为现有标准最大残留限量值的制(修)订提供科学依据。方法:以乙腈为溶媒,对收集的16批三七进行高速匀浆法提取处理;针对拟定的检测指标,分别采用气相色谱串联质谱法(GC-MS/MS)和高效液相色谱串联质谱法(HPLC-MS/MS)、多反应监测(MRM)模式进行检测,以不少于2组特征离子对进行定性,并采用校准曲线法对检出农药进行定量检测;结合本课题组前期建立的风险评估方法,对检出率较高的高风险农药进行暴露评估,计算其急性和慢性摄入风险。结果:所建方法共有262个农药指标(总计271个化合物),在线性范围内线性关系良好,灵敏度、回收率均符合痕量多残留分析技术要求。16批三七样品中共检出50种农药,农药检出率较高,多数检出农药处于痕量水平,仅百菌清、毒死蜱、三氟氯氰菊酯、异菌脲、五氯硝基苯、甲基硫菌灵超出团体标准《无公害三七药材及饮片农药与重金属及有害元素的最大残留限量》(T/CATCM 003—2017)的最大残留限量(MRL)。水洗可明显降低部分检出农药的残留量。对超出限量标准,以及无相关限量标准但检出率较高的农药品种进行风险评估,结果显示,9种农药的短期危害指数(HIa)为0.0002~0.1418、长期危害指数(HIc)为0.0004~0.0090,其中五氯硝基苯的HIa和HIc较高,但风险可接受。结论:建立了三七中262种农药多残留筛查方法,并采用暴露评估方法中的点评估模式对其进行健康风险评估,可为三七相关农药残留限量标准的制修订提供参考。

Screening and Risk Assessment of 262 Pesticide Residues in Notoginseng Radix et Rhizoma

Objective To screen and assess the levels of multiple pesticide residues in Notoginseng Radix et Rhizoma and evaluate the intake exposure of the highly detected pesticide residues, so as to provide a scientific basis for the revision of the maximum residue limits (MRL) in existing standards.Methods A total of 16 batches of Notoginseng Radix et Rhizoma samples were extracted by high-speed homogenate with acetonitrile as solvent. Their pesticide residues were analyzed by GC-MS/MS and HPLC-MS/MS in MRM mode. No less than two groups of characteristic ion pairs were selected for qualitative detection, and the calibration curve method was used for quantitative detection of pesticide residues. Finally, combined with the risk assessment method established by the research group, the exposure assessment of high-risk pesticides with a high detection rate was carried out. The acute and chronic intake risks were calculated.Results A total of 262 pesticide indicators (involving 271 chemical monomers) were used in the established method. The linear relationship was good in the linear range, and the sensitivity and recovery rate met the technical requirements of multiple residue trace analysis. 50 pesticides were detected in 16 batches of Notoginseng Radix et Rhizoma samples, and the detection rate of pesticides was higher. Most of the detected pesticides were at the trace level, and only chlorothalonil, chlorpyrifos, cyfluthrin, isometrin, pentachloronitrobenzene, and methyl thiobacillin exceeded the MRL in group standard Maximum Residue Limits of Pesticides, Heavy Metals, and Harmful Elements for Non-Pollution Notoginseng Radix Herbs and Decoction Pieces (T/CATCM 003-2017). In addition, water washing could significantly reduce the residual amount of some detected pesticides. Risk assessment was carried out for pesticide varieties exceeding MRL or pesticides with a high detection rate. The results showed that the short-term hazard index (HIa) and long-term hazard index (HIc) of nine pesticides were 0.000 2-0.141 8 and 0.000 4-0.009 0, respectively. Among them, the HIc and HIa of pentachloronitrobenzene were high, with acceptable risks.Conclusion In this study, screening methods for 262 pesticide residue in Notoginseng Radix et Rhizoma were established, and the health risk assessment was conducted by using the point assessment model of exposure assessment, which could provide a reference for improving the revision of pesticide residue limit standards in Notoginseng Radix et Rhizoma.