超高效液相色谱—三重四极杆质谱法测定黄瓜中双炔酰菌胺残留

Determination of mandipropamid residues in cucumber by UPLC-MS

目的:建立一种超高效液相串联三重四极杆质谱检测黄瓜中双炔酰菌胺含量的方法。方法:黄瓜试样经乙腈超声提取后,采用分散固相萃取法(QuEChERS)进行净化,超纯水稀释,用0.1%甲酸水和乙腈作为流动相进行液相色谱—串联质谱测定。采取电喷雾(ESI)离子源在正离子检测模式下,对双炔酰菌胺进行多反应监测(MRM),并使用外标法进行定量。结果:在0.01~0.50μg/mL质量浓度范围内,双炔酰菌胺具有良好的线性关系,R^(2)=0.9998;在10,50,100 mg/mL 3种不同加标水平下,双炔酰菌胺回收率为89.6%~96.0%,相对标准偏差(RSD)为0.72%~1.80%(n=6)。试验方法检出限为0.003 mg/kg;定量限为0.009 mg/kg。结论:试验方法前处理过程无需浓缩,操作简便,分析灵敏度高、稳定性好、重现性高,适用于黄瓜中双炔酰菌胺的定性与定量分析。

Objective:To establish a detecting method for mandipropamid residues in cucumber by UPLC-MS coupled with the positive ions mods of MRM.Methods:The cucumber samples were was extracted by ultrasonic acetonitrile and then were purified by dispersed solid phase extraction(QuEChERS).Cucumber solution diluted with ultrapure water,and filtered by 0.22μm water phase.Then 0.1%formic acid water(A)and acetonitrile(B)were used as mobile phase for isocratic elution.Results:The results showed that a good linearity was obtained for the standard curve of the method,its correlation was high,R^(2)=0.9998.Its detection limit was 0.003 mg/kg,and its limit of quantification was 0.009 mg/kg.Meanwhile,its recovery rate was between 89.6%~96.0%at the three levels of 10,50 and 100 mg/mL.Conclusion:The method is simple,sensitive and reproducible.This method is suitable for qualitative and quantitative analysis of mandipropamid in cucumber,and it is a suitable method for rapid determination of mandipropamid in cucumber.