【摘要】：血清中的電解質(zhì)是骨骼和細(xì)胞健康的重要標(biāo)志物,監(jiān)測其濃度水平的變化常通過分析血清中鉀、鈣、鎂和鋰的含量來實(shí)現(xiàn)。雖然傳統(tǒng)的同位素稀釋-熱電離質(zhì)譜法(ID-TIMS)作為基準(zhǔn)參考方法在準(zhǔn)確性和溯源性上一直領(lǐng)航于許多二級參考方法,但其冗長而繁瑣的樣品前處理操作過程,在某種程度上阻礙了此方法在常規(guī)臨床檢測中的廣泛應(yīng)用。本研究主要包括如下內(nèi)容：(1)通過向血清中人為添加電解質(zhì)的氯化物溶液實(shí)現(xiàn)三個水平的血清標(biāo)準(zhǔn)物質(zhì)中電解質(zhì)的濃度呈現(xiàn)高、中、低梯度分布,所選擇的特性量值元素為：鉀、鈣、鈉、鎂、鋰和氯；(2)對比研究了H2和NH3兩種碰撞反應(yīng)氣消除ICP-MS測量鉀、鈣、鎂和鋰時的質(zhì)譜干擾情況,并通過引入四種元素混合標(biāo)準(zhǔn)樣品溶液,對射頻功率、碰撞氣流速、RPq等參數(shù)進(jìn)行實(shí)驗(yàn)優(yōu)化,得到了最佳的測量條件；(3)建立了同位素稀釋-電感耦合等離子體質(zhì)譜法(ID-ICP-MS),結(jié)合“冷”等離子體和碰撞反應(yīng)池兩種模式,同時加入41K、42Ca、25Mg和6Li四種同位素稀釋劑溶液,且同時測定鉀、鈣、鎂和鋰的含量。這一方法既省去了樣品前處理過程中繁瑣的基體分離步驟,又消除了質(zhì)譜測量過程中Ar基分子離子的干擾,實(shí)現(xiàn)了人血清中鉀、鈣、鎂和鋰含量的準(zhǔn)確測定；(4)使用NIST冷凍人血清電解質(zhì)標(biāo)準(zhǔn)物質(zhì)SRM956c level2、LGC冷凍人血清標(biāo)準(zhǔn)物質(zhì)ERM-DA250a和中國計量科學(xué)研究院冷凍人血清中無機(jī)成份分析標(biāo)準(zhǔn)物質(zhì)GBW09152共三款標(biāo)準(zhǔn)物質(zhì)驗(yàn)證所建立的方法,其中鉀、鈣、鎂和鋰的測定結(jié)果與標(biāo)準(zhǔn)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.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：R446.1

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