人体血清标准物质中无机成份定值分析方法研究

发布时间：2019-02-13 15:56

【摘要】：血清中的电解质是骨骼和细胞健康的重要标志物,监测其浓度水平的变化常通过分析血清中钾、钙、镁和锂的含量来实现。虽然传统的同位素稀释-热电离质谱法(ID-TIMS)作为基准参考方法在准确性和溯源性上一直领航于许多二级参考方法,但其冗长而繁琐的样品前处理操作过程,在某种程度上阻碍了此方法在常规临床检测中的广泛应用。本研究主要包括如下内容：(1)通过向血清中人为添加电解质的氯化物溶液实现三个水平的血清标准物质中电解质的浓度呈现高、中、低梯度分布,所选择的特性量值元素为：钾、钙、钠、镁、锂和氯；(2)对比研究了H2和NH3两种碰撞反应气消除ICP-MS测量钾、钙、镁和锂时的质谱干扰情况,并通过引入四种元素混合标准样品溶液,对射频功率、碰撞气流速、RPq等参数进行实验优化,得到了最佳的测量条件；(3)建立了同位素稀释-电感耦合等离子体质谱法(ID-ICP-MS),结合“冷”等离子体和碰撞反应池两种模式,同时加入41K、42Ca、25Mg和6Li四种同位素稀释剂溶液,且同时测定钾、钙、镁和锂的含量。这一方法既省去了样品前处理过程中繁琐的基体分离步骤,又消除了质谱测量过程中Ar基分子离子的干扰,实现了人血清中钾、钙、镁和锂含量的准确测定；(4)使用NIST冷冻人血清电解质标准物质SRM956c level2、LGC冷冻人血清标准物质ERM-DA250a和中国计量科学研究院冷冻人血清中无机成份分析标准物质GBW09152共三款标准物质验证所建立的方法,其中钾、钙、镁和锂的测定结果与标准值相符性良好。
[Abstract]:Electrolytes in serum are important markers of bone and cell health. Monitoring the concentration of electrolytes is usually achieved by analyzing the contents of potassium, calcium, magnesium and lithium in serum. Although the traditional isotope dilution / thermoelectric ionization mass spectrometry (ID-TIMS) method has been used as a reference method for reference in accuracy and traceability, it has been used in many secondary reference methods, but it is a long and tedious sample pretreatment process. To some extent, it hinders the wide application of this method in routine clinical detection. The main contents of this study are as follows: (1) the concentration of electrolyte in three levels of serum standard substances is high, medium and low gradient distribution is achieved by adding chloride solution artificially to the serum. The selected characteristic values are: potassium, calcium, sodium, magnesium, lithium and chlorine; (2) the interference between H _ 2 and NH3 collision gas in ICP-MS measurement of potassium, calcium, magnesium and lithium by mass spectrometry was studied. The radio frequency power and the impact flow velocity were determined by introducing four elements into the standard sample solution. RPq and other parameters are optimized by experiments, and the optimal measurement conditions are obtained. (3) Isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS) was established, combined with "cold" plasma and collision reaction cell, and four isotopic diluents (41kg ~ (42) Ca ~ (2 +) mg and 6Li) were added at the same time. The contents of potassium, calcium, magnesium and lithium were also determined. This method not only eliminates the tedious steps of matrix separation in sample pretreatment, but also eliminates the interference of Ar molecular ions in mass spectrometry, and realizes the accurate determination of potassium, calcium, magnesium and lithium in human serum. (4) using NIST to freeze human serum electrolyte standard material SRM956c level2,LGC to freeze human serum standard material ERM-DA250a and Chinese Academy of metrology to freeze human serum inorganic component analysis standard material GBW09152 three standard materials were established to verify. The results of determination of potassium, calcium, magnesium and lithium are in good agreement with the standard values.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：R446.1

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