LC-MS/MS测定婴幼儿配方乳粉中2种全氟化合物

Determination of Two Kinds of Perfluorinated Compounds in Infant Formula Milk Powder by LC-MS/MS

建立SCIEX QTRAP 5500 LC-MSMS测定婴幼儿配方乳粉中全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS)的方法。试验利用优化后的方法同时测定样品中全氟辛酸和全氟辛烷磺酸的残留,内标法定量。结果表明,在优化试验条件下,各物质的线性关系良好,线性范围分别为PFOA 0.05~1.0 ng/mL和PFOS 0.5~10 ng/mL,相关性均在0.999以上,方法检出限分别为PFOA 0.002μg/kg和PFOS 0.02μg/kg。在3种加标量水平下,回收率达到93.0%~101.1%, 3种加标量PFOA为0.01, 0.02和0.10μg/kg, PFOS为0.10, 0.20和1.00μg/kg,方法精密度SRSD为1.5%~4.2%(n=6)。该方法操作简单快速,灵敏度高,能满足婴幼儿配方乳粉样品中PFOA和PFOS的同时测定。

To establish a method for the determination of perfluorooctanoate(PFOA) and perfluorooctane sulfonate(PFOS) in infant formula milk powder by SCIEX QTRAP 5500 LC-MS/MS, the samples needed to be determined and confirmed by the method which instrumental parameters were optimized, and quantified by internal standard method. The results showed that standard curves were obtained with correlation coefficients greater than 0.999. The linear ranges of PFOA were 0.05-1.0 ng/m L and PFOS were 0.5-10 ng/mL. The detection limits of the method of PFOA was 0.002 μg/kg and PFOS was 0.02 μg/kg;The spike recoveries at three different replicates of PFOA 0.01, 0.02 and 0.10 μg/kg, and PFOS 0.10, 0.20 and 1.00 μg/kg were 93.0%-101.1% with SRSD varying from 1.5%-4.2%(n=6). The method was simple, rapid and sensitive. Perfluorooctanoate(PFOA) and Perfluorooctane sulfonate(PFOS) in infant formula milk powder could be determined simultaneously by this method.