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目的:建立采用电感耦合等离子体质谱(ICP-MS)法测定中药材侧柏叶中18种重金属及微量元素(Pb,TI,Hg,Dy,Ba,Sb,Sn,Cd,Ag,Mo,Se,As,Cu,Ni,Mn,Cr,Al,Be,Ge,In)的方法,该方法的建立对全面修订完善侧柏叶质量标准,提高侧柏叶质量控制水平提供实验基础。方法:侧柏叶样品经微波消解后,18种元素中质量数小于100的元素采用Ge作为内标,质量数大于100的元素采用In作为内标,采用ICP-MS法进行测定。结果:检测的Pb,TI,Hg,Dy,Ba,Sb,Sn,Cd,Ag,Mo,Se,As,Cu,Ni,Mn,Cr,Al,Be 18种元素线性关系良好,相关系数R2≥0.974 6,各元素的检出限在0.224~1.792μg·L~(-1),回收率在81.0%~117.1%。测定来自不同产地63批侧柏叶样品,Hg,Cu,Cd,Sb 4种元素的量均较低,As均未检出,Ba有部分样品超出限度要求,Pb绝大部分样品超出限度要求,Al超出限度范围较高,分析测定结果,Ni,Cr,Mn,Al,Cu,Ba是侧柏叶无机元素的主成分,可作为特征元素,来自不同产区的侧柏叶样品表现出一定的聚类性特征。结论:建立的方法操作简便,分析速度快,灵敏度高,内标法更能提高测定结果的精密度和准确性,该方法适用于中药材侧柏叶中重金属及微量元素的测定。
Objective: To establish a method for the determination of 18 heavy metals and trace elements in P. orientalis leaves by inductively coupled plasma mass spectrometry (ICP-MS). (Pb,TI,Hg,Dy,Ba,Sb,Sn,Cd,Ag,Mo,Se The method for the preparation of As, Cu, Ni, Mn, Cr, Al, Be, Ge, In), the establishment of the method provides an experimental basis for the comprehensive revision and improvement of the quality standard of Platycladus orientalis leaves and the improvement of the quality control of Platycladus orientalis leaves. METHODS: After microwave digestion of P. orientalis leaves, Ge was used as the internal standard in the elements with the mass of less than 100, and In was used as the internal standard in the elements with the mass greater than 100. The determination was carried out by ICP-MS. Results: The detected Pb,TI,Hg,Dy,Ba,Sb,Sn,Cd,Ag,Mo,Se,As,Cu,Ni,Mn,Cr,Al,Be 18 elements have a good linear relationship, the correlation coefficient R2≥ 0.974 6, the detection limit of each element was 0.224~1.792μg·L~(-1), and the recovery rate was 81.0%~117.1%. Determination of 63 samples of P. orientalis leaves from different producing areas showed that the amounts of Hg, Cu, Cd, and Sb elements were all low, As was not detected, some Ba samples exceeded the limit, and most Pb samples exceeded the limits. The Al out-of-limit range is higher. Analysis results show that Ni, Cr, Mn, Al, Cu and Ba are the main components of the inorganic elements of Platycladus orientalis leaves, and can be used as characteristic elements. The samples of P. orientalis from different producing areas show a certain degree. Clustering features. Conclusion: The established method is easy to operate, with fast analysis speed and high sensitivity. The internal standard method can improve the precision and accuracy of the measurement results. This method is suitable for the determination of heavy metals and trace elements in the Chinese herbal medicine P. orientalis.