直接稀释-电感耦合等离子体质谱法测定母乳中17种元素的含量  

Determination of 17 Elements in Breast Milk by Inductively Coupled Plasma Mass Spectrometry with Direct Dilution

作　　者：孙琦[1] 尹晋 唐永春 胡小键[1] 朱英[1] SUN Qi;YIN Jin;TANG Yongchun;HU Xiaojian;ZHU Ying(China CDC Key Laboratory of Environment and Population Health,National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,Beijing 100021,China;Physical and Chemical Department of Health Inspection and Testing Center,Qinghai Province Disease Prevention Control Center,Xining 810007,China)

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

出　　处：《理化检验（化学分册）》2024年第9期878-884,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：中央财政经费资助项目(131031108000150003)。

摘　　要：提出了直接稀释-电感耦合等离子体质谱法(ICP-MS)同时测定母乳中钒、铬、锰、钴、镍、铜、锌、砷、硒、锶、钡、钼、镉、锡、锑、汞、铅等17种元素含量的方法。取母乳0.5 mL,用含2%(体积分数)硝酸和0.01%(体积分数)四甲基氢氧化铵的0.01%(体积分数)曲拉通X-100溶液定容至10 mL,涡旋混匀,以转速4000 r·min^(-1)离心5 min,将上清液用0.45μm水相滤膜过滤,在动能歧视(KED)模式下采用ICP-MS测定滤液中上述17种元素的含量,在线加入含6μg·L^(-1)钪、锗、铑、铋的混合内标使用液。结果表明:各元素的质量浓度在一定范围内与所对应的信号强度与内标元素信号强度比呈线性关系,检出限(3s)为0.019~0.768μg·L^(-1);方法用于分析美国国家标准参考材料,除锌元素外,其他元素的测定值均在认定值的不确定度范围内,并且日内和日间的变异系数均小于13%;按照标准加入法进行回收试验,回收率为81.3%~119%。A method for simultaneous determination of 17 elements including vanadium,chromium,manganese,cobalt,nickel,copper,zinc,arsenic,selenium,strontium,barium,molybdenum,cadmium,tin,antimony,mercury,and lead in breast milk by inductively coupled plasma mass spectrometry(ICP-MS)with direct dilution was proposed.0.5 mL of breast milk was taken and made its volume up to 10 mL with 0.01%(volume fraction)Triton X-100 solution containing 2%(volume fraction)nitric acid and 0.01%(volume fraction)tetramethyl ammonium hydroxide.The mixture was vortex mixed evenly,and centrifuged at a rotational speed of 4000 r·min^(-1)for 5 min.The supernatant solution was passed through a 0.45μm water phase filter membrane,17 elements in the filtrate were determined by ICP-MS in kinetic energy discrimination(KED)mode,and 6μg·L^(-1)mixed internal standard solution,including scandium,germanium,rhodium,and bismuth was added online.As shown by the results,linear relationships between the ratios of the corresponding signal intensity to the internal standard signal intensity and mass concentrations of elements were found in definite ranges,with detection limits(3s)in the range of 0.019-0.768μg·L^(-1).This method was used for analysis of American national standard reference materials,and the determined values of other elements except zinc were found within the uncertainty range of the certified values,with coefficients variation of intra-day and inter-day less than 13%.Test for recovery was made by the standard addition method,giving results in the range of 81.3%-119%.

关 键 词：直接稀释 电感耦合等离子体质谱法(ICP-MS) 母乳 元素 

分 类 号：O657.63[理学—分析化学]