母乳中16种元素的石墨消解-碰撞模式-电感耦合等离子体-质谱测定法  

Determination of 16 elements in breast milk by graphite digestion,collision mode,inductively coupled plasma-mass spectrometry

作　　者：唐永春 莫延慧 胡小键[2] 张续[2] 朱英[2] 孙琦[2] TANG Yong-chun;MO Yan-hui;HU Xiao-jian;ZHANG Xu;ZHU Ying;SUN Qi(Physical and Chemical Department of Inspection and Testing Center,Qinghai Center for Disease Control and Prevention,Xining,Qinghai 810007,China;不详)

机构地区：[1]青海省疾病预防控制中心检验检测中心理化科,西宁810007 [2]中国疾病预防控制中心环境与人群健康重点实验室,中国疾病预防控制中心环境与健康相关产品安全所,北京100021

出　　处：《环境与健康杂志》2024年第9期804-809,共6页Journal of Environment and Health

基　　金：中国疾控中心环境所环境污染健康影响人体生物监测体系(131031108000150003)。

摘　　要：目的建立母乳中钒、铬、锰、钴、镍、铜、锌、砷、硒、锶、钡、钼、镉、锡、锑、铅16种元素的石墨消解-碰撞模式(KED)-电感耦合等离子体质谱(ICP-MS)测定方法。方法使用石墨消解仪对母乳进行消解,以2.5 ml硝酸+0.5 ml双氧水为消解液,在150℃下消解45 min,在100℃赶酸30 min后,得到0.5 ml溶液,使用ICP-MS仪的KED模式测定样品中的16种元素。结果在0.05~2000μg/L范围内,所得16种元素的回归方程的线性关系良好,r>0.999。该方法的检出限为0.04~5μg/L,定量下限为0.1~15μg/L。各元素的批内及批间变异系数(CV)在0.5%~11.3%之间,加标回收率在81.6%~118%之间。结论该方法的线性范围宽、检出限低、灵敏度高、准确性良好、操作安全,适用于母乳中16种元素的测定。Objective To develop a method for the determination of 16 elements in breast milk by graphite digestion,collision mode(KED),inductively coupled plasma-mass spectrometry(ICP-MS).Methods Breast milk was digested by using a graphite digester with 2.5 ml of nitric acid+0.5 ml of hydrogen peroxide as the digesting solution.The solution was digested at 150℃for 45 min,and then the acid was driven off at 100℃for 30 min to obtain a 0.5 ml solution,which was used to determine 16 elements in the samples by using the KED mode of the ICP-MS instrument,namely vanadium,chromium,manganese,cobalt,nickel,copper,zinc,arsenic,selenium,strontium,barium,molybdenum,cadmium,tin,antimony and lead.Results The linearity of the regression equations for the 16 elements was good in the 0.05-2000μg/L range,with r>0.999.The limits of detection(LOD)of the method were in the range of 0.04-5μg/L,and the lower limits of quantification(LOQ)were in the range of 0.1-15μg/L.The coefficients of variation(CV)for each element were in the range of 0.5%-11.3%,and the recoveries were in the range of 81.6%-118%.Conclusion The method has a wide linear range,low detection limit,high sensitivity,good accuracy,safe operation,and it is applicable to the determination of 16 elements in breast milk.

关 键 词：母乳 元素 石墨消解 电感耦合等离子体-质谱 

分 类 号：O657.6[理学—分析化学]