超临界流体萃取气相色谱法测定鱼肉中的毒死蜱残留

Determination of Chlorpyrifos in Fish Tissue bySupercritical Fluid Extraction and Gas Chromatography

建立了利用离线超临界CO2萃取气相色谱(SFE-GC)测定鱼肌肉中毒死蜱残留量的分析方法.超临界CO2萃取鱼肌肉中毒死蜱的适宜条件为: 温度100℃,压力41.370 MPa,CO2流量为1 mL/min,动态萃取30 min,静态萃取时间15 min,调节剂甲醇(添加量0.5 mL),收集液丙酮.最小检出量为0.01 ng;添加回收率为77.3%～105.1%;相对标准偏差(RSD)为2.4%～15.4%,符合残留分析要求.全程分析时间小于2 h.

The insecticide chlorpyrifos was extracted from fish tissue by supercritical fluid extraction (SFE). The extraction conditions were optimized, including temperature, pressure, modifier, and collection solvent. Gas chromatography with electron-capture detection was used to analyse the extracts. The analytes were extracted at 41370 kPa and 100° C with 1 mL/min supercritical carbon dioxide modified with methanol for 30 min after 15 min static extraction. The extracts were collected in 20 mL of acetone. Recoveries ranged from 77.3% ∼ 105.1%, and a method precision of 2. 4% ∼ 15.4% was obtained for spiking levels of 1 ∼ 10 mg/kg.