4种小作物中嘧菌酯残留量的检测及膳食风险评估

Determination of azoxystrobin residue in 4 kinds of minor crops and dietary risk assessment

中文关键词:  嘧菌酯  4种小作物  残留  超高效液相色谱-串联质谱法  风险评估

英文关键词:azoxystrobin  4 kinds of minor crops  residue  ultra performance liquid chromatography-tandem mass spectrometer  risk assessment

中文摘要:

      目的 建立超高效液相色谱-串联质谱联用法检测4种小作物(茄子、苦瓜、葱和蕹菜)中嘧菌酯残留的分析方法, 探明嘧菌酯在4种小作物中的残留特性和使用安全性。方法 样品经乙腈提取, QuEChERS方法净化, 在电喷雾正离子(electrospray positive ion, ESI+)模式下, 用UPLC-MS/MS采用多反应监测(multiple reaction monitoring, MRM)模式检测。结果 嘧菌酯在0.001~2 mg/L浓度范围内溶剂标准曲线和空白基质匹配标准曲线均有良好线性, 相关系数在0.9989~1之间。在0.01~20 mg/kg 添加水平内平均回收率为73.5%~109.7%, 相对标准差(relative standard deviation, RSD)为1.5%~8.9%, 方法的检出限(limits of detection, LOD)为0.001 mg/L, 最低检测浓度(limits of quantification, LOQ)为0.01 mg/kg。25%嘧菌酯水分散粒剂在4种小作物中的半衰期分别为3.9、2.7、4.6和2.5 d; 连续多次施药10 d后在茄子和苦瓜中残留量最大值分别为0.015 mg/kg和0.018 mg/kg; 连续多次施药14 d后在葱和蕹菜中残留量最大值分别为1.43 mg/kg和 0.450 mg/kg; 膳食风险商值(risk quotient, RQ)为0.0002~0.0959, 均低于1。结论 该方法简便 、快速、灵敏度高, 能有效克服杂质干扰, 膳食风险结果表明使用25%嘧菌酯水分散粒剂防治蔬菜病害风险较小, 相对安全。

英文摘要:

      Objective To establish a method for the determination of azoxystrobin residue in four kinds of minor crops (eggplant, bitter gourd, scallions and water spinach) by ultra performance liquid chromatography-tandem mass spectrometry, and investigate the residual properties and safety of azoxystrobin. Methods The samples were extracted with acetonitril, and cleaned-up by QuEChERS. Then, the residues of azoxystrobin were analyzed by ultra performance liquid chromatography-tandem mass spectrometer (UPLC/MS/MS), under electrospray positive ion using multiple reaction monitoring (MRM) mode. Results The azoxystrobin had high correlation coefficients at the range of 0.001-2 mg/L, with the correlation coefficients between 0.9989 and 1. When the spiked levels of 0.01 20 mg/kg in 4 kinds of minor crops, the spiked recoveries of azoxystrobin in all samples were between 73.5%109.7%, with the relative standard deviation (RSD) between 1.5% to 8.9%. The detection limit of quantification was 0001%. The results indicated that the half-lives of 25% azoxystrobin in four kinds of minor crops were 3.9, 2.7, 4.6 and 2.5 days, respectively. The ?nal residues in eggplant and bitter gourd were 0.015 mg/kg and 0.018 mg/kg after 10 days of continuous application. The ?nal residues in scallions and water spinach were 1.43 mg/kg and 0.450 mg/kg after 14 days of contimuous application. The maximum value at risk quotient of azoxystrobin were 0.0002-0.0959, both lower than 1. Conclusion This method is simple, rapid, sensitive, and can effectively overcome the interference of impurities. The dietary risk assessment results show that 25% azoxystrobin water dispersible granule is relatively safe and less risk for vegetable disease control.