加速溶剂萃取-气相色谱法检测鱼粉中7种指示性多氯联苯方法研究

Study on the method for detecting 7 kinds of indicative polychlorinated biphenyls in fish meal by accelerated solvent extraction-gas chromatography

中文关键词:  鱼粉  多氯联苯  加速溶剂萃取法  气相色谱法

英文关键词:fish meal  polychlorinated biphenyls  accelerated solvent extraction  gas chromatography

中文摘要:

      目的 建立采用加速溶剂萃取-气相色谱检测鱼粉中7种指示性多氯联苯残留的方法。方法 采用加速溶剂萃取法, 以正己烷-二氯甲烷(1:1, V:V)为提取剂对鱼粉样品进行提取, 提取温度为120 ℃, 压力为10 MPa, 静态提取时间为8 min, 循环提取2次。用浓硫酸进行净化后, 用气相色谱法进行分析测定。结果 多氯联苯在5~500 ng/mL浓度范围内线性关系良好, 相关系数为0.9986~0.9999, 方法定量限为3.0~5.0 μg/kg, 3个添加水平的平均回收率为85.5%~104%, 相对标准偏差为2.61%~8.26%。结论 本方法精密度好, 准确度高, 操作简单、快速, 适用于鱼粉中多氯联苯的定量检测。

英文摘要:

      Objective To establish a method for detecting 7 kinds of indicative polychlorinated biphenyls (PCBs) residues in fish meal by accelerated solvent extraction-gas chromatography (ASE-GC). Methods The PCBs were extracted with n-hexane-methylene chloride (1:1, V:V) by ASE with the extraction temperature at 120 ℃, pressure at 10 MPa, and the static extracting time at 8 min. The above operating steps were repeated twice. After being purified by concentrated sulfuric acid, the extract was analyzed by GC. Results The PCBs had good linearities at the range of 5~500 ng/mL, the correlation coefficients were 0.9986~0.9999, and the limit of quantification were 3.0~5.0 μg/kg. The average recovery rates of the PCBs in 3 spiked levels ranged from 85.5% to 104% with the relative standard deviations (RSDs) were 2.61%~8.26%. Conclusion The proposed method was precise, accurate, simple and rapid, which is suitable for the quantitative detection of PCBs in fish meal.