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采用粉末压片制样,实现了螺旋藻中磷、硫、氯、溴、硅、钠、钾、镁、钙、钛、钒、铬、铁等23种微量元素的X射线荧光光谱法测定。研究了粉末压片法制样时研磨时间和颗粒度对荧光响应信号的影响,采用GBW07603,GBW10025等国家一级标准物质绘制校准曲线,经标准物质验证,分析结果与标样吻合。对样品中23种元素所测值做精密度考察,同一样片重复测定10次时各元素含量的相对标准偏差在0.7%~10%范围内;10个样片分别测试时各元素含量的相对标准偏差在0.1%~6.6%范围内。通过与电感耦合等离子体质谱法比对,所得结果基本一致。研究表明,X射线荧光光谱法可以实现螺旋藻中一系列微量元素的便捷、准确检测。
X-ray fluorescence spectrometry was established for the determination of 23 trace elements of phosphorus, sulfur, chlorine, bromine, silicon, sodium, potassium, magnesium, calcium, titanium, vanadium, chromium and iron in Spirulina with powder tabletting. The effects of grinding time and particle size on the fluorescence response signal were studied. The calibration curves of GBW07603, GBW10025 and other national standard materials were drawn. The calibration curves were verified by the standard materials. The analytical results were in good agreement with the standard samples. The relative standard deviation (RSD) of the content of each element in the same sample was measured in 10% range from 0.7% to 10%. The relative standard deviations In the range of 0.1% ~ 6.6%. By inductively coupled plasma mass spectrometry comparison, the results are basically the same. Studies have shown that X-ray fluorescence spectrometry can be a convenient and accurate detection of a series of trace elements in Spirulina.