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    ICP-MS/ICP-AES测定矿物药龙骨中55种元素的含量及龙骨来源的鉴别

    Determination of 55 Elements in Mineral Medicine Os Draconis by ICP-MS/ICP-AES and Identification of Os Draconis Sources

    • 摘要: 取0.1 g龙骨样品粉末置于聚四氟乙烯消解管中,加入5 mL硝酸,密封混匀,于220 ℃微波消解30 min,冷却,加少量水润洗并转移至50 mL容量瓶中,用水定容,离心。采用电感耦合等离子体原子发射光谱法(ICP-AES)测定上清液中P、S元素的含量,电感耦合等离子体质谱法(ICP-MS)联合内标法测定其余53种元素的含量。运用IBM SPSS Statistics 26.0软件对37批龙骨样品中检出的51种元素进行相关性分析,SIMCA14.1软件识别龙骨的来源及引起差异的元素。结果表明,P、S元素的质量浓度在一定范围内和对应的信号强度呈线性关系,其余53种元素的质量浓度在一定范围内和对应的信号强度与内标信号强度的比值呈线性关系,检出限(3s)为0.000 2~7.916 mg·kg−1。对实际龙骨样品溶液进行精密度试验,测定值的相对标准偏差(n=6)均小于13%。按照标准加入法进行回收试验,回收率为85.0%~114%。方法用于分析37批实际龙骨样品,结果显示龙骨中Ca、P元素含量最高且之间呈显著正相关,Ba、Na、Mg、S、Al、Sr、Fe等元素在不同批次中含量差异较大且元素之间存在不同程度相关,重金属及有害元素含量相对较低,Te、Os、Ru、Pt等元素均未检出;U、Sr、Mg及稀土元素可能是引起不同来源龙骨差异的标志性元素。

       

      Abstract: The Os Draconis sample powder (0.1 g) was taken and placed in a polytetrafluoroethylene digestion tube, and 5 mL of nitric acid was added. The mixture was sealed and thoroughly mixed, and digested by microwave at 220 ℃ for 30 min. After cooling down, a small amount of water was added to rinse, and the solution was transferred into a 50 mL-volumetric flask and made its volume up to 50 mL with water. The solution was centrifuged, and P and S elements in the supernatant were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), and the remaining 53 elements were determined by inductively coupled plasma mass spectrometry (ICP-MS) with internal standard method. The 51 elements detected in 37 batches of Os Draconis samples were subjected to the correlation analysis using the IBM SPSS Statistics 26.0 software, and the SIMCA14.1 software was used for identification the sources of Os Draconis and elements that caused the differences. As shown by the results, linear relationships between the corresponding signal intensities and mass concentrations of P and S elements were kept in definite ranges, and linear relationships between the ratios of the corresponding signal intensity to the internal standard signal intensity and mass concentrations of the remaining 53 elements were kept in definite ranges, with detection limits (3s) in the range of 0.000 2-7.916 mg·kg−1. Test for precision was conducted on actual Os Draconis sample solutions, with RSDs (n=6) of the determined values less than 13%. Test for recovery was made by the standard addition method, giving results in the range of 85.0%-114%. This method was applied to analysis of 37 batches of actual Os Draconis samples, and it was shown by the results that the contents of Ca and P elements in Os Draconis were the highest, and there was a significant positive correlation between them. The contents of Ba, Na, Mg, S, Al, Sr, and Fe elements were varied greatly among different batches, and there were varying degrees of correlation between them. The contents of heavy metals and harmful elements were relatively lower. Te, Os, Ru, and Pt elements were not detected. U, Sr, Mg, and rare earth elements might be characteristic elements that caused the differences among Os Draconis from different sources.

       

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