毛细管气相色谱法测定保健食品、中药材中的五氯硝基苯残留

DETERMINATION OF QUINTOZENE RESIDUES IN HEALTH FOOD AND CHINESE HERBAL DRUGS BY CAPILLARY GAS CHROMATOGRAPHY

建立保健食品中五氯硝基苯残留量的毛细管气相色谱检测方法。样品经正己烷超声提取,硫酸净化,采用分流不分流进样方式,用弱极性毛细柱程序升温分离,电子俘获检测器检测,外标法定量。五氯硝基苯浓度在0.005～0.10μg/mL范围内与峰面积线性相关,线性相关系数r=0.9996,方法检出限为0.0006 mg/kg。0.02 mg/kg和0.05 mg/kg两水平添加量的回收率为93.0%～94.5%,测定结果的相对标准偏差分别为1.20%、2.79%(n=6)。被测样品中存在不同程度的五氯硝基苯残留。本法操作简便,分离效果及重复性好。

The quintozene residues in health food and Chinese herbal drugs was determined by capillary gas chromatography. The quintozene in sample was extracted by ultrasonication with n-hexane, purified with sulfuric acid and injected with split/splitless mode. The capillary column was HP -5 with programmed increasing temperature. The quintozene residues were detected with electron capture detector and calculated by external standard method. The peak area was linear with the concentration of quintozene in the range of 0. 005 - 0.10 μg/mL,r = 0.999 6. The detection limit was 0. 000 6 mg/kg. The recoveries were 93.0% and 94.5%. The RSD was less than 3 % （n = 6）. The tested health food and Chinese herbal drugs contained quintozene residues in different levels. This method is easy in operation and good in separation and repeatability.