同位素稀释离子色谱-串联质谱法同时测定食品中的氯酸盐和高氯酸盐

Simultaneous determination of chlorate and perchlorate in food by isotope dilution ion chromatography-tandem mass spectrometry

中文关键词:  离子色谱-串联质谱法  高氯酸盐  氯酸盐  食品

英文关键词:ion chromatography-tandem mass spectrometry  perchlorate  chlorate  food

中文摘要:

      目的 建立一种同位素稀释离子色谱-串联质谱法测定食品中氯酸盐和高氯酸盐含量的分析方法。 方法 一般试样经0.2%乙酸水溶液提取, 含乳样品加入乙酸锌溶液和亚铁氰化钾溶液进行沉淀, C18-SPE小柱净化, 离子色谱-串联质谱法测定, 内标法定量。结果 高氯酸盐在0.015~10 μg/L浓度范围内有良好的线性关系, 相关系数r>0.999, 检出限为0.5 μg/kg, 定量限为1.5 μg/kg, 加标回收率为80.0~101%, 相对标准偏差(relative standard deviation, RSD)小于6.0%, 氯酸盐在0.05~20 μg/L浓度范围内有良好的线性关系, 相关系数r>0.999, 检出限为1.5 μg/kg, 定量限为5.0 μg/kg, 加标回收率在80.0%~97.1%, 相对标准偏差(relative standard deviation, RSD)小于6.0%。结论 该方法简便、可靠、稳定, 可用于各类食品中高氯酸盐和氯酸盐含量的快速测定与确认。

英文摘要:

      Objective To establish a method for determination of perchlorate and chlorate in food by isotope dilution ion chromatography-tandem mass spectrometry. Methods General samples were extracted by 0.2% acetic acid solution, the emulsion samples were precipitated by adding zinc acetate solution and potassium ferrous cyanide solution. The samples were purified by C18-SPE column, detected by ion chromatography-tandem mass spectrometry and quantified by the internal standards solution. Results Perchlorate had a good linear relationship in the range of 0.015-10 μg/L, with r>0.999, the limit of detection was 0.5 μg/kg, the limit of quantification was 1.5 μg/kg, the recoveries were 80.0%-101%, and the relative standard deviation (RSD) was less than 6.0%. The chlorate had a good linear relationship in the range of 0.05-20 μg/L, with r>0.999. The limit of detection was 1.5 μg/kg, the limit of quantification was 5.0 μg/kg, the recoveries were 80.0%~97.1%, and the RSD was less than 6.0%. Conclusion This method is simple, rapid and accurate, which is suitable for the determination of perchlorate and chlorate in food.