SPE-GC/MS 法分析鱼塘水中的5种农药

摘要

目的：建立鱼类中毒案件中鱼塘水5种农药的固相萃取（solid phase extraction，SPE）结合气相色谱－质谱联用仪（GC/MS）的检测方法。方法比较 Oasis HLB cartridge、Bond Elut C18和 SampliQ C183种固相萃取柱提取、净化鱼塘水中5种农药的提取回收率，并考察洗脱剂种类、洗脱剂用量对提取回收率的影响。结果利用 Bond Elut C18固相萃取柱，以3mL 苯作为洗脱剂，鱼塘水中5种农药质量浓度在1~50μg/mL范围内有良好的线性关系，相关系数为0．9962~0．9996，测得的检出限为3．4~26μg/L，提取回收率为61．49%~102．48%，相对标准偏差均≤3．01%。结论 SPE－GC/MS 法灵敏度高、准确度和精密度好，简单快速，溶剂消耗量少，适用于鱼塘水中5种农药的检测。%Objective To establish the solid phase extraction (SPE) with GC/MS technology for fish poi-soning cases to determine five pesticides in fishpond. Methods By three solid phase extraction column including Oasis HLB cartridge, Bond Elut C18 and SampliQ C18, the recovery rate was compared to ex-tract and purify five pesticides in fishpond. The effects of different kinds and dosages of eluents on ex-tract rate were also reviewed. Results Using Bond Elut C18 as solid phase extraction column and 3 mL benzene as eluent, the linear range of mass concentration of five pesticides in fishpond was 1-50 μg/mL, and the correlation coefficient was 0.996 2-0.999 6. The limit of detection was 3.4-26 μg/L and the re-covery was 61.49%-102.48%. The relative standard deviations was less than or equal to 3.01%. Conclu-sion With high sensitivity, good accuracy and precision, SPE -GC/MS has simple and quick operation and less solvent. It can be applied to determination of five pesticides in fishpond.