以晚熟杂柑品种“沃柑”为研究对象,采用超高效液相色谱-串联质谱法分析了三唑磷、丙溴磷、毒死蜱和联苯菊酯4种常用杀虫杀螨剂的残留消解规律及最终残留量,评估其潜在膳食风险。结果表明,建立的方法线性、灵敏度、准确度和精密度良好,相关系数≥0.99,定量限为10 μg/kg,回收率为74.1%~100.6%,相对标准偏差在0.5%~13.5%,能满足沃柑中4种农药的残留检测要求。三唑磷、丙溴磷、毒死蜱和联苯菊酯在沃柑上的消解规律符合一级动力学方程,半衰期分别为21.7~30.1、22.4~28.9、13.9~15.4和19.8~24.8 d,降解速率较慢,在果实中的最终残留除了毒死蜱可降解到其最大残留限量值(maximum residue limit,MRL)以下外,三唑磷、丙溴磷和联苯菊酯均超出其各自的MRL。4种杀虫杀螨剂残留主要集中在果皮中,果肉中残留对人体的健康风险可忽略不计,但整个果实中残留的三唑磷对儿童和一般人群以及联苯菊酯对儿童的急性膳食摄入风险值超出了可接受范围,存在急性健康风险。果实转色期后应停止使用三唑磷、丙溴磷和联苯菊酯,不建议对沃柑整个果实或果皮产品进行加工食用。研究结果可为我国沃柑质量安全生产、监测和消费引导提供技术参考。
The dissipation behavior, final residues and potential dietary risks of four commonly used insecticides and acaricides (triazophos, profenofos, chlorpyrifos and bifenthrin) were determined by liquid chromatography-tandem mass spectrometry technology with a late hybrid variety ‘Orah mandarin’ as the research object. The results showed that satisfactory results of good linearity (r≥0.99), sensitivity (limits of quantification 10 μg/kg), recoveries (74.1%-100.6%) with relative standard deviations (0.5%-13.5%) were obtained in the method validation, which could meet the requirements for the determination of the four pesticide residues in Orah mandarin. The half-lives of triazophos, profenofos, chlorpyrifos and bifenthrin in Orah mandarin were 21.7-30.1 d, 22.4-28.9 d, 13.9-15.4 d and 19.8-24.8 d, respectively according to first-order kinetics. The final residues of triazophos, profenofos and bifenthrin were all above their MRLs with a slow dissipation rate. Only residual concentration of chlorpyrifos was below its MRL at pre-harvest interval. Residues of the four pesticides were mainly found in peels and the health risks of four pesticide residues in Orah flesh were negligible low. However, the potential acute dietary exposure risks of triazophos to children and general population and bifenthrin to children from Orah whole fruits were unacceptable. Therefore, the use of triazophos, profenofos and bifenthrin after fruit color break period should be prohibited. It is advisable to avoid consuming the processed products from the whole fruits or peels of Orah mandarins. The results of this study can provide a technical reference for the safe production, monitoring and consumption guidance of Orah mandarins in China.
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