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,C_(18)-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0.015~10μg/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0.5μg/kg,定量限为1.5μg/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0.05~20μg/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1.5μg/kg,定量限为5.0μg/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。
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 vg/L, with r〉0.999, the limit of detection was 0.5 μg/kg, the limit of quantification was 1.5μg/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%. Conelusion This method is simple, rapid and accurate, which is suitable for the determination ofperchlorate and chlorate in food.
作者
孙文闪
周敏
刘芯成
王川丕
SUN Wen-Shan;ZHOU Min;LIU Xin-Cheng;WANG Chuan-Pi(Greentown Agricultural Testing Technology Co.,Ltd.,Hangzhou 310000,China)
出处
《食品安全质量检测学报》
CAS
2018年第14期3679-3685,共7页
Journal of Food Safety and Quality
关键词
离子色谱-串联质谱法
高氯酸盐
氯酸盐
食品
ion chromatography-tandem mass spectrometry
perchlorate
chlorate
food
