摘要
采用离子色谱-串联质谱法测定婴幼儿配方奶粉中的高氯酸盐。将2.00g样品溶解在10mL水中,加入乙腈10mL,振荡离心去除样品中的蛋白质,上清液用10mL乙腈饱和的正己烷溶液去除样品中的脂类物质。净化液采用Dionex IonPac AS 20色谱柱分离,以60mmol·L^(-1)氢氧化钾溶液洗脱。质谱中采用电喷雾离子源和多反应监测模式,以NaCl 18O4作为同位素内标物质定量。高氯酸盐质量浓度的线性范围为0.1~100μg·L^(-1),检出限(3S/N)为0.3μg·kg^(-1),测定下限(10S/N)为1.0μg·kg^(-1)。加标回收率在92.1%~97.0%之间,测定值的相对标准偏差(n=6)小于10%。
IC-MS/MS was applied to the determination of perchlorate in infant formula. 2.00 g of the sample was dissolved in 10 mL of water, and then the solution was mixed well with 10 mL of acetonitrile. The mixture was centrifuged to eliminate the protein, and the lipids in the supernatant were eliminated with 10 mL of acetonitrile saturated hexane. The purified solution was separated on a Dionex IonPac AS 20 chromatographic column with 60 mmol . L -1 KOH solution as the eluent. ESI and MRM were adopted in MS and NaCl18 04 was used as the isotope internal standard for quantification. Linear relationship was found between the peak area and the mass concentration of perchlorate in the range of 0. 1-100μg . L -1 , with detection limit （3S/N） of 0. 3 μg .kg- 1 and the lower limit of determination （10S/N） of 1.0 μg . kg -1. Recovery rates obtained by standard addition method were in the range of 92. 1μ-97.0μ, and RSDs （n=6） were less than 10%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2016年第1期19-23,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局科技项目(2013QK136)
