UPLC-MS/MS同时检测婴幼儿配方乳粉中氯酸盐和高氯酸盐残留

Simultaneous determination of chlorate and perchlorate residues in infant milk powder by UPLC-MS/MS

该实验建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定婴幼儿配方乳粉中氯酸盐和高氯酸盐残留量的方法。样品经甲酸水提取,乙腈沉淀蛋白,乙腈饱和正己烷除去脂肪,采用Anionic Polar Pesticide色谱柱(2.1 mm×150 mm,5μm)分离,以0.9%甲酸+50 mmol/L甲酸铵水溶液和乙腈为流动相梯度洗脱,在电喷雾离子源负离子(ESI-)多反应监测模式条件下,对氯酸盐和高氯酸盐进行定性和定量分析。结果表明,高氯酸盐和氯酸盐分别在0.5~50.0μg/L和1.0~100.0μg/L范围内线性关系良好,高氯酸盐和氯酸盐的定量限(LOQ)分别为7.5μg/kg和15.0μg/kg。高氯酸盐和氯酸盐的加标回收率为82.5%~98.5%,精密度试验结果的相对标准偏差(RSD)为2.0%~8.7%;该方法稳定、准确、灵敏度高,可用于婴幼儿配方乳粉中氯酸盐和高氯酸盐残留量检测。

In this experiment,an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for simultaneously quantitative determination of chlorate and perchlorate in infant milk powder.The samples were extracted by formic acid water and protein was precipitated by acetonitrile.Using acetonitrile saturated n-hexane to remove fat,and the analytes were separated by Anionic Polar Pesticide column(2.1 mm×150 mm,5μm),eluted by gradient with 0.9%formic acid solution+50 mmol/L ammonium formate aqueous solution and acetonitrile.Mass spectrometry conditions were scanned by electron spray ionization(ESI-)multiple reaction monitoring(MRM)mode to conduct qualitative and quantitative analysis of the chlorate and perchlorate residues.The results showed that perchlorate and chlorate demonstrated good linearity at 0.5-50.0μg/L and 1.0-100.0μg/L,respectively.The limit of quantitation(LOQ)of perchlorate and chlorate were 7.5μg/kg and 15.0μg/kg,respectively.The recoveries of perchlorate and chlorate were 82.5%-98.5%,respectively.The relative standard deviation(RSD)of precision tests result were 2.0%-8.7%.The method was stable,accurate and with high sensitivity,which could be used for the chlorate and perchlorate determination in infant milk powder.