CI-LLME萃取技术在果蔬多种杀菌剂残留分析中的应用

Application of CI-LLME Extraction Technology in Residue Analysis of Various Fungicides in Fruits and Vegetables

目的:建立CI-LLME-超高效液相色谱-串联质谱法检测果蔬中8种杀菌剂残留量的方法。方法:使用冷冻诱导液液微萃取前处理技术结合三重四极杆分析技术检测果蔬产品中8种杀菌剂的残留量。结果:在给定的浓度范围内8种杀菌剂存在良好的线性关系(R2>0.990);方法检出限为0.04~1.83μg·kg^(-1),定量限为0.12~5.49μg·kg^(-1)。10.0μg·L^(-1)、20.0μg·L^(-1)、100.0μg·L^(-1)添加水平的回收率为81.5%~117.1%,精密度(RSD)为0.05%~6.12%,重复性实验标准偏差为0.045~0.887,RSD为0.47%~9.47%,均符合国家标准要求。结论:该前处理技术具备一步式样品前处理能力,简单快速、成本较低,灵敏度高且重现性好,因此该技术可用于检测果蔬中多种微量杀菌剂的含量。

Objective:To create a method for detecting the residues of eight fungicides in fruits and vegetables using CI-LLME-ultra high performance liquid chromatography-tandem mass spectrometry.Method:The residue of eight fungicides in fruit and vegetable products was detected using liquid-liquid freeze-induced liquid-liquid microextraction pre-treatment technology combined with triple quadrupole analysis technology.Result:Good linear relationships(R2>0.990)were observed for the eight fungicides in the given concentration ranges;the limits of detection of the method were in the range of 0.04~1.83μg·kg^(-1),and the limits of quantification of the method were in the range of 0.12~5.49μg·kg^(-1).The recoveries were in the range of 81.5%~117.1%at the spiked levels of 10.0μg·L^(-1),20.0μg·L^(-1),100.0μg·L^(-1) and precision of the method was in the range of 81.5%~117.1%,the precision(RSD)was 0.05%~6.12%,and the standard deviation of repeatability experiment was 0.045~0.887 with the RSD of 0.47%~9.47%.Conclusion:This pre-treatment technology has the capability of one-step sample pretreatment,which is simple,fast,cost-effective,sensitive,and reproducible.Therefore,this technology can be used to detect the content of various trace fungicides in fruits and vegetables.