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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10MPa,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3.0~5.0μg/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。
Objective To establish a method for the determination of seven indicated PCBs in fishmeal using accelerated solvent extraction - gas chromatography. Methods Accelerated solvent extraction was used to extract fishmeal from n-hexane-methylene chloride (1: 1, V: V). The extraction temperature was 120 ℃, the pressure was 10 MPa and the static extraction time was 8 min. Extract 2 times. After purifying with concentrated sulfuric acid, it was analyzed by gas chromatography. Results The linearity of PCBs ranged from 5 ng / mL to 500 ng / mL with a correlation coefficient of 0.9986 to 0.9999 with a limit of quantification of 3.0-5.0 μg / kg. The average recovery of PCBs was 85.5% 104%, relative standard deviation of 2.61% ~ 8.26%. Conclusion The method has good precision, high accuracy, simple and fast operation, and is suitable for the quantitative detection of PCBs in fishmeal.