电感耦合等离子体质谱法测定藠头17种元素的方法探讨

目的建立藠头中Li、Al、V、Cr、Mn、Fe、Ni、Cu、Zn、As、Se、Cd、Sn、Sb、Ba、Hg和Pb共17种元素的电感耦合等离子体质谱(ICP-MS)测定方法。方法选择微波消解法,并对检测方法的条件进行优化,称样量为1 g(精确至0.0001 g),80℃赶酸至消解液剩余1 mL,用重量法定容,双曲线同时测定,以内标元素进行校正,采用ICP-MS法同时测定藠头中的17种元素。结果测定的各元素线性关系良好,r为0.9991~1.0000,各元素的检出限为0.0008~0.1 mg/kg,精密度、重复性和重现性试验的相对标准偏差(RSD)均符合定量分析要求;加标回收率为81.0%~118.3%,RSD为0.2%~8.7%,标准物质测定值均在标准值允许的范围。结论通过对方法前处理条件及检测进行优化,降低误差,达到提高实验结果准确度和精密度以及检测效率的效果。方法学考察表明,该方法简便快速、准确、灵敏、重现性好,适用于同时测定藠头中17种元素。

The determination of 17 elements in Allium chinense G.Don was performed by inductively coupled plasma mass spectrometry

Objective To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of Li,Al,V,Cr,Mn,Fe,Ni,Cu,Zn,As,Se,Cd,Sn,Sb,Ba,Hg and Pb in Allium chinense G.Don.Methods Microwave digestion method was used and the detection conditions were optimized.The sample size was 1 g(accurated to 0.0001 g),and the acid was pumped at 80℃to the remaining 1 ml of the digestive juice.Determine the volume by weight,simultaneously measured by hyperbola,calibrated with internal standard elements,and ICP-MS method was used to simultaneously determine 17 elements in Allium chinense.Results The linear relationship of all elements measurement was good,with r between 0.9991-1.0000,and the detection limit of each element was between 0.0008-0.1 mg/kg.The RSD of precision,repeatability,and reproducibility tests all met the requirements of quantitative analysis.The standard recovery was 81.0%-118.3%,RSD was 0.2%-8.7%,and the measured values of the standard substances were all within the allowable range of the standard values.Conclusion This article optimizes the pre-processing conditions and detection methods to reduce errors,which achieves the effect of improving the accuracy and precision of the experimental results and improving the detection efficiency.The method is simple,rapid,accurate,sensitive,and reproducible.It is suitable for the simultaneous determination of 17 elements in Allium chinense G.Don.