优化液质法测定多种基质中五氯酚残留量

LC-MS for the Determination of Pentachlorophenol Residues in a Variety of Matrices

在GB 23200.92-2016《动物源性食品中五氯酚残留量的测定液相色谱-质谱法》的基础上,改进了前处理方法,使用1%氨水乙腈提取,QuEChERS法净化,氮吹后甲醇复溶,并在多种基质中进行了方法学验证。结果表明,方法平均回收率为72.22%~89.51%;精密度试验中,相对标准偏差(RSD)为4.23%~10.28%(n=6);在1~10μg/L范围内线性关系良好(相关系数r>0.995);加标量为1.0μg/kg的情况下,信噪比>10;定量限小于1.0μg/kg,满足检测需求。该方法能够节省前处理时间,同时降低成本。

On the basis of GB 23200.92-2016"Determination of pentachlorophenol residues in foods of animal origin liquid chromatography-mass spectrometry",the pretreatment conditions were improved,using 1%ammonia water and acetonitrile to extract,QuEChERS method to purify,methanol after nitrogen blowing reconstitute.The results showed that the method could pass the methodological verification in various matrices,and the average recovery rate was 72.22%~89.51%.The precision test was performed separately,and the relative standard deviation(RSD)was 4.23%~10.28%(n=6),the linear relationship in the range(1~10μg/L)is outstanding(correlation coefficient R>0.995),the quantification limit is 1.0μg/kg,and the signal-to-noise ratio is greater than 10.The method can save the time spent on pretreatment,and reduce some costs.