运用电感耦合等离子体原子发射光谱法进行生物医用钽和钛材料的成分分析

Composition Analysis of Biomedical Tantalum and Titanium Materials by Inductively Coupled Plasma Atomic Emission Spectrometry

目的从医疗器械生物学评价和生产监管的角度,采用电感耦合等离子体原子发射光谱法(ICP-OES)建立生物医用钽(Ta)、钛(Ti)材料的成分分析方案。方法样品经超声消解后转移至容量瓶中,定容得到样品溶液;利用ICP-OES氢氟酸系统对样品溶液中的34种元素进行预筛,并对筛选后的元素进行方法学考察;通过对Ti合金标准物质的比对测试,对该检测方法进行验证。结果对预筛后的Ta、Ti、铌(Nb)、钼(Mo)、锌(Zn)、硅(Si)、钨(W)、铅(Pb)等18种元素进行了方法学考察,结果均满足检验要求。其中Ta、Ti主含量元素检出限分别为11.40、109.80 ng/ml,其余16种元素的检出限均低于15 ng/ml;所测元素的精密度在2%以内,2 h的变化率均小于11%,平均回收率为85%~112%。Ti合金比对测试结果符合GB/T 3620.2-2007《钛及钛合金加工产品化学成分允许偏差》的规定要求,证明了该检测方法的可靠性。结论运用ICP-OES建立生物医用Ta、Ti材料的成分分析方案可行,可用来明确Ta、Ti材料的组分含量,评估医疗器械的安全风险。

Objective For the purpose of biological evaluation and production supervision of medical devices,inductively coupled plasma atomic emission spectrometry(ICP-OES method)was used to explore and establish a composition analysis scheme for biomedical tantalum(Ta)and titanium(Ti)materials.Methods After ultrasonic digestion,samples were transferred to volumetric flasks to obtain the sample solutions at constant volume.The 34 elements in the sample solutions were screened by ICP-OES of hydrofluoric acid resistant system,and the methodology of the screened elements were investigated.The test method was verified by comparing with the standard material of Ti alloy.Results 18 elements[such as Ti,Ta,niobium(Nb),molybdenum(Mo),zinc(Zn),silicon(Si),tungsten(W),lead(Pb),etc.]which were screened out were investigated by methodology,and all the results could meet the test requirements.The limits of detection of the major elements Ti and Ta were 11.40 and 109.80 ng/ml,and the remaining 16 elements were all lower than 15 ng/ml.The precision of the measured elements was less than 2%,the rate of change within 2 h was less than 11%,and the average recovery was between 85%and 112%.The comparative determination results of Ti alloy conformed to GB/T 3620.2-2007 Titanium and titanium alloys——permissible variations of chemical composition for wrought product analysis,which proved the reliability of the analysis method.Conclusion It is feasible to establish the component analysis scheme of biomedical Ta and Ti materials by ICP-OES method,which can be used to determine the component content of Ta and Ti materials and evaluate the safety risks of medical devices.