荔枝中3种杀虫剂的残留行为及膳食风险评估

Residues behavior and dietary risk assessment of 3 kinds of pesticides in Litchi chinensis

目的建立超高效液相色谱-串联质谱法(ultra performance liquidchromatography-tandem mass spectrometry,UPLC-MS/MS)测定荔枝中3种杀虫剂(虱螨脲、除虫脲和氯虫苯甲酰胺)残留的分析方法,并研究3种杀虫剂在荔枝中的残留行为及其膳食风险评估。方法荔枝中残留的3种杀虫剂采用乙腈提取,UPLC-MS/MS检测,基质匹配外标法定量。根据残留检测结果和我国不同人群的膳食消费量评估膳食风险。结果在0.0005~0.0500mg/L范围内,峰面积和浓度呈良好线性关系,相关系数均大于0.999;虱螨脲、除虫脲和氯虫苯甲酰胺在荔枝中平均回收率范围分别为81%~97%、77%~105%和73%~102%,最大相对标准偏差为14.2%,定量限均为0.010mg/kg。结果表明,虱螨脲、除虫脲和氯虫苯甲酰胺在荔枝中半衰期分别为6.3~21.8、6.3~22.1和3.9~10.6 d。膳食风险评估表明,3种杀虫剂的膳食风险商均远小于1。结论该方法简便、准确、灵敏度高,可用于荔枝中虱螨脲、除虫脲和氯虫苯甲酰胺的残留检测。于安全间隔期(14 d)时采收的荔枝样品中,除虫脲和氯虫苯甲酰胺的最终残留量均低于我国相应的最大残留限量值(0.5mg/kg和1.0mg/kg),我国尚未制定虱螨脲在荔枝中的最大残留限量。经过风险评估,3种杀虫剂在荔枝中的残留不会对不同人群健康产生不可接受的风险。

Objective To establish a method for the determination of 3 kinds of insecticides(lufenuron,diflubenzuron and chlorantraniliprole)residues in Litchi chinensis based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),and study the residual behavior and dietary risk assessment of 3 kinds of pesticides in Litchi chinensis.Methods Three pesticides in Litchi chinensis were extracted with acetonitrile,detected by UPLC-MS/MS and quantified with matrix matched external standard method.The dietary risks to different subgroups of Chinese were assessed according to the results of the experiments.Results In the range of 0.0005 to 0.0500 mg/L,the peak area showed a good linear relationship with its mass concentration,and the correlation coefficient was greater than 0.999.Meanwhile,the average recoveries of lufenuron,diflubenzuron and chlorantraniliprole were 81%–97%,77%–105%and 73%–102%with the maximum relative standard deviations of 14.2%in Litchi chinensis,respectively.The limits of quantification were 0.010 mg/kg.The results showed that the half lives of lufenuron,diflubenzuron and chlorantraniliprole in Litchi chinensis were 6.3–21.8 d,6.3–22.1 d and 3.9–10.6 d,respectively.The dietary risk assessment indicated that the risk quotient of 3 kinds of pesticides were far below 1.Conclusion The method is simple,accurate and sensitive,and can be used for the residue determination of lufenuron,diflubenzuron and chlorantraniliprole residues in Litchi chinensis.The final residue level of diflubenzuron and chlorantraniliprole in harvest does not exceed the maximum residue limits in China of 0.5 mg/kg and 1.0 mg/kg,respectively,after 14 days of the last application.The maximum residue limit of lufenuron in Litchi chinensis was not established by China.After the risk assessment,the residue of 3 kinds of pesticides in Litchi chinensis will not pose an unacceptable risk to the health of different population.