摘要:
针对生物样品的特殊性,本文建立了微波消解—电感耦合等离子体发射光谱同时测定生物样品中铝(Al)、铁(Fe)、镁(Mg)、钙(Ca)、钠(Na)、钾(K)、锰(Mn)、磷(P)、钛(Ti)、钡(Ba)、锶(Sr)、锌(Zn)等12种元素的分析方法。通过对微波消解样品前处理条件进行优化,选择以10 mL逆王水和1 mL双氧水的混合试剂作为消解试剂,并选择合适的微波消解仪实验程序,能保证样品分解完全;选择最优的等离子体激发条件、元素分析谱线及扣背景位置,使得各元素测定的灵敏度高以及谱线无干扰;以国家一级生物成分标准物质作为校准系列绘制校准曲线,使得校准系列与试样基体尽可能一致,且选定方法总稀释倍数为100,消除了基体效应干扰影响。结果表明:该方法检出限为(0.04~4.93)×10-6;方法相对标准偏差(RSD)为1.41%~5.13%,精密度较好;经国家一级生物成分标准物质验证,方法相对误差(RE)均在±10%以内,测定值与标准值相吻合,方法准确可靠,能够满足生物样品分析要求。
Abstract:
Given the particularity of biological samples, this study employed microwave digestion and inductively coupled plasma-optical emission spectrometry (ICP-OES) for the simultaneous determination of 12 elements in biological samples, including aluminum (Al), ferrum (Fe), magnesium (Mg), calcium (Ca), sodium (Na), potassium (K), manganese (Mn), phosphorus (P), titanium (Ti), barium (Ba), strontium (Sr), and zinc (Zn). By optimizing the pretreatment conditions of microwave digestion samples, this study selected the mixed reagent of reverse aqua regia (10 mL) and hydrogen peroxide (1 mL) as the digestion reagent, and an appropriate experimental procedure for the microwave digestion system to ensure complete decomposition of samples. Moreover, this study selected the optimal plasma excitation conditions, analytical spectral lines of elements, and background subtraction position to ensure high determination sensitivity of elements and interference-free spectral lines. This study plotted the calibration curve with the national primary reference materials for biological components as the calibration series, making the calibration series consistent with the sample matrix as much as possible. The simultaneous determination method had a total dilution multiple of 100, eliminating the interference of the matrix effect. The results show that this method had a detection limit of (0.04~4.93)×10-6 and a relative standard deviation (RSD) of 1.41%~5.13%, showing high precision. As verified by the national primary reference materials, this method had a relative error (RE) within ±10% and determined values consistent with standard values. Therefore, this method is accurate and reliable, meeting the analysis requirements of biological samples.
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