全反射X射线荧光光谱法快速测定全血中多种无机元素的含量  

Rapid Determination of Multiple Inorganic Elements in Whole blood by Total Reflection X-Ray Fluorescence Spectrometry

作　　者：高捷[1] 朱月琴 屈海云[1] 盛成[1] 钱荣[1] 卓尚军[1] GAO Jie;ZHU Yueqin;QU Haiyun;SHENG Cheng;QIAN Rong;ZHUO Shangjun(Inorganic Materials Analysis and Testing Center,The Shanghai Institute of Ceramics of the Chinese Academy of Sciences,Shanghai 201899,China)

机构地区：[1]中国科学院上海硅酸盐研究所无机材料分析测试中心,上海201899

出　　处：《理化检验（化学分册）》2024年第6期561-565,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点研发计划(2021YFF0700104);上海无机材料测试技术平台(19DZ2290700)。

摘　　要：为实现全血样品中无机元素的快速、准确测定,提出了题示方法。取经乙二胺四乙酸(EDTA)抗凝处理过的全血样品100 mg和100 mg·L^(−1)镓内标溶液10 mg,分别用100 mg、500 mg、1000 mg 1%(质量分数)Triton X-100溶液(稀释剂)(对应稀释剂和样品质量比1∶1,5∶1,10∶1,记作“稀释比”)进行分散,混匀后振荡2 min,采用全反射X射线荧光光谱仪检测,结合内标法和相对灵敏度因子公式计算全血样品中无机元素的含量。结果显示:加大稀释比有利于磷、硫、钾、钙元素的分散,有助于提高其测定结果的准确度;采用相对灵敏度因子校正可将磷、硫元素的回收率提高至80.0%以上;方法应用于豚鼠全血样品的分析,检出了磷、硫、钾、钙、铁、铜、锌、铷、硒等无机元素。和电感耦合等离子体原子发射光谱法(ICP-AES)相比,这9种元素测定值的相对误差的绝对值均小于10%,测定值的相对标准偏差(n=20)不大于18%;7种元素(铷、硒除外)的检出限(3s)为0.2~19 mg·L^(−1)。该方法无需消解样品和制作标准曲线,可在25 min内完成全血样品分析。The method mentioned by the title was proposed to achieve rapid and accurate determination of inorganic elements in whole blood samples.An aliquot(100 mg)of the whole blood sample treated by ethylenediaminetetraacetic acid(EDTA)anticoagulation was taken,and 10 mg of 100 mg·L^(−1) gallium internal standard solution and 1%(mass fraction)Triton X-100 solution(diluent)of 100 mg,500 mg or 1000 mg(corresponding diluent to sample mass ratios of 1∶1,5∶1,10∶1,referred to as“dilution ratio”)were added for dispersion.After mixing and shaking for 2 min,the resulting solution was detected by total reflection X-ray fluorescence spectrometer.The content of inorganic elements in the whole blood sample was calculated using the relative sensitivity factor calculation formula conmined with internal method.It was shown that increasing the dilution ratio was beneficial for the dispersion of phosphorus,sulfur,potassium and calcium elements,which helped to improve the accuracy of their determination results.The use of relative sensitivity factor correction could increase the recovery of phosphorus and sulfur elements to over 80.0%.The proposed method was used for analyzing guinea pig sample,and inorganic elements of phosphorus,sulfur,potassium,calcium,iron,copper,zinc,rubidium and selenium were detected.Compared with inductively coupled plasma atomic emission spectrometry,absolute values of the relative errors of the determined values for the 9 inorganic elements were less than 10%,and RSDs(n=20)of the determined values were not greater than 18%.The detection limits(3s)of 7 elements(except rubidium and selenium)was 0.2-19 mg·L^(−1).The method did not require sample digestion or standard curve production,and could complete the whole blood sample analysis within 25 min.

关 键 词：全反射X射线荧光光谱法(TXRF) 全血 无机元素 快速分析 

分 类 号：O657.34[理学—分析化学]