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

作　　者：徐敦明[1] 陈安良[1] 余向阳[1] 王箐霞[1] 何军[1] 张兴[1] 

机构地区：[1]西北农林科技大学无公害农药研究服务中心,杨凌712100

出　　处：《分析化学》2005年第4期451-454,共4页Chinese Journal of Analytical Chemistry

基　　金：国家"十五"攻关资助项目(No. 2002BA516A04)

摘　　要：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.

关 键 词：超临界流体萃取 毒死蜱 气相色谱法 测定 超临界CO2萃取 鱼肉 相对标准偏差 CO2流量 适宜条件 萃取时间 残留分析 分析时间 鱼肌肉 残留量 min 添加量 调节剂 检出量 回收率 甲醇 丙酮 集液 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]