离子色谱串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐

Determination of chlorate and perchlorate in infant formula milk powder by ion chromatography tandem mass spectrometry

中文关键词:  氯酸盐  高氯酸盐  离子色谱法  串联质谱法  婴幼儿配方奶粉

英文关键词:chlorate  perchlorate  ion chromatography  tandem mass spectrometry  infant formula milk powder

中文摘要:

      目的 建立离子色谱串联质谱法(ion chromatography tandem mass spectrometry, IC-MS/MS)检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的分析方法。方法 样品经提取、净化除去蛋白质及脂类物质后, 采用离子色谱法分离, 电喷雾串联质谱法测定, 并采用氯酸盐-18O3和高氯酸盐-18O4作为同位素内标物质进行定量。结果 在10 min内完成了氯酸盐和高氯酸盐的分离分析。氯酸盐和高氯酸盐在低中高3个添加水平的回收率为79.7%~96.4%, 相对标准偏差小于5%(n=6), 氯酸盐检出限为1.0 μg/kg, 高氯酸盐检出限为0.3 μg/kg。结论 该方法准确、可靠, 可同时检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的含量。

英文摘要:

      Objective To establish a method for determination of chlorate and perchlorate in infant formula milk powder by ion chromatography tandem mass spectrometry (IC-MS/MS). Methods The sample was extracted, purified to remove the protein and fat material, then separated by IC, and determined by electrospray ionization tandem mass spectrometry, with 18O3 chlorate and 18O4 perchlorate used as isotopic internal standard for quantitative analysis. Results The separation and analysis of chlorate and perchlorate were completed within 10 min. The recoveries were ranged from 79.7% to 96.4% for chlorate and perchlorate at 3 spiked levels. The relative standard deviations (RSDs) were less than 5% (n=6), and the limits of detection(LODs) for chlorate and perchlorate were 1.0 μg/kg and 0.3 μg/kg, respectively. Conclusion This method is accurate and reliable, which is suitable for the determination of chlorate and perchlorate in infant formula milk powder.