氟菌唑及其代谢物在葡萄中的动态残留分析及膳食风险评估

Dynamic residue analysis and dietary risk assessment of fluconazole and its metabolites in Vitis vinifera

目的探究30%氟菌唑可湿性粉剂在葡萄中的残留及消解动态,并评估膳食摄入风险。方法葡萄园内选3个试验小区内不同时期的葡萄,经乙腈提取、盐析、CaptivaEMR-GPF净化后,利用气相色谱-三重四极杆质谱法多重反应离子监测模式进行定性定量分析氟菌唑及其代谢物残留量及消解动态实验,并进行摄入膳食风险评估。结果氟菌唑及其代谢物在葡萄中的检出限为0.001 mg/kg,平均回收率为82.1%~90.4%,相对标准偏差2.04%~3.96%。氟菌唑及其代谢物在葡萄中的半衰期分别为1.1~1.2 d和1.9~2.9 d。不论以低剂量还是高剂量,施药后30d,氟菌唑及其代谢物在葡萄样品中最终残留量均低于0.3mg/kg。膳食风险评估表明,施药15 d后,不同人群膳食摄入风险概率均小于100%。结论该方法简单、准确、灵敏度高,适用于葡萄中氟菌唑及其代谢物的残留检测。最终结果表明,葡萄中氟菌唑及其代谢物的残留量未超过标准规定临时限量,施药15 d后产生的膳食风险可接受。

Objective To investigate the residue and degradation dynamics of 30%fluconazole wettable powder in Vitis vinifera,and evaluate the dietary intake risk.Methods Vitis vinifera from different stages in 3 experimental plots were selected in the vineyard.After extraction with acetonitrile,salt precipitation,and purification with Captiva EMR-GPF,qualitative and quantitative analysis of fluconazole and its metabolites residues and degradation dynamics were conducted using gas chromatography-triple quadrupole mass spectrometry with multiple reaction ion monitoring mode.Dietary risk assessment was also conducted.Results The limit of detection of fluconazole and its metabolites in Vitis vinifera was 0.001 mg/kg,the average recovery rates were 82.1%-90.4%,relative standard deviations were 2.04%-3.96%.The half-lives of fluconazole and its metabolites in Vitis vinifera are 1.1 to 1.2 days and 1.9 to 2.9 days,respectively.Regardless of whether at low or high doses,the final residual amount of fluconazole and its metabolites in grape samples was less than 0.3 mg/kg 30 days after application.The dietary risk assessment showed that after 15 d of application,the probability of dietary intake risk for different populations was less than 100%.Conclusion This method is simple,accurate,and highly sensitive,and is suitable for the residual detection of fluconazole and its metabolites in Vitis vinifera.The final results indicate that the residual levels of fluconazole and its metabolites in Vitis vinifera do not exceed the temporary limit specified by the standard,and the dietary risk generated after 15 days of application is acceptable.