果蔬中6种杀真菌剂残留的固相分散气相色谱检测及基质效应

Matrix Solid-phase Dispersion and Gas Chromatographic Analysis and Matrix Effect in Determination of 6 Fungicides Residues in Fruits and Vegetables

采用基质固相分散样品前处理技术,气相色谱-电子捕获检测器测定果蔬中残留的常用杀真菌剂--五氯硝基苯(PCNB)、五氯苯胺(PCA)、甲基五氯苯基硫醚(MPCS)、腐霉利(PRO)、克菌丹(CAP)和异菌脲(IPR)。对影响提取效果的参数,如吸附剂类型、提取溶剂、超声波辅助提取等工艺条件进行优化。利用空白基质配制标准样品溶液来补偿和消除色谱分析中存在的基质效应,结果表明,该方法的回收率在78.4%～109.7%,相对标准偏差低于10%,检测限0.1～0.4μg/kg。该方法可用于水果、蔬菜中杀真菌剂残留量的测定。

A rapid method based on matrix solid-phase dispersion was developed for the determination of pen- tachloronitrobenzene （PCNB）, pentachloraniline （PCA）, methyl-pentachlorophenyl sulfide （MPCS）, procymidone （PRO）, captan（CAP） and Iprodione（IPR） in fruits and vegetables. After the optimisation of different parameters such as the type of adsorbent, the extraction solvent, and the extraction assistance by sonication. The analysis of samples was accom- plished using gas chromatography with electron-capture detector（GC-ECD）. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The results showed the recoveries of the method were in the range 78.4%-109.7%, and with relative standard deviations lower than 10%. The limits of detections ranged from 0.1-0.4μg/kg. The proposed methods were applied to the analysis of these compounds in fruits and vegeta- bles samples.