微波消解-电感耦合等离子体质谱法(ICP-MS)测定蛇床子中16种稀土元素

Determination of 16 rare earth elements in Cnidii Fructus by ICP-MS

目的:建立电感耦合等离子体质谱法(ICP-MS)同时测定蛇床子中16种稀土元素(钪、钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥)的含量。方法:蛇床子(12批)经微波消解后采用ICP-MS测定,射频功率为1 300 W,采样深度为6.8 mm,辅助气、等离子体气和载气流速分别为1.0、16.0和1.17 L·min^(-1),雾化室温度为2℃;通过在线加入内标铼(Re)和铑(Rh)元素的方法来校正基质效应和干扰。结果:各元素在各自检测质量浓度范围内线性关系良好(r均不低于0.999 3),检出限为0.03~0.32μg·kg^(-1),回收率为90.1%~105.7%,重复性RSD值为0.9%~3.1%。不同产地的蛇床子中各元素含量差别较大。结论:经方法学验证,本法可用于蛇床子中16种稀土元素的检测,为其质量控制提供参考依据。

Objective： To establish a method for the determination of 16 rare earth elements （Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu）in Cnidii Fructus by inductively coupled plasma mass spectrometry （ICP-MS）.Methods： The total 12 batches of Cnidii Fructus were collected.Samples were digested by microwave and measured with ICP-MS.The RF power was 1 300 W, and the sampling depth was 6.8 mm.The flow rate of auxiliary gas, plasma gas and carrier gas were 1.0, 16.0 and 1.17 L·min-1, respectively.The atomizing chamber temperature was 2℃.The internal standard solution with Re and Rh were used to correct the interference of matrix elements and spectra.Results： The validated method indicated that the linearity was good and the correlative coefficients （r）for the 16 rare earth elements were all above 0.999 3.The limits of detection were in the range of 0.03 to 0.32 μg·kg-1.The recoveries of elements were between 90.1% and 105.7%.The precision were good with RSD in the range of 0.9% to 3.1%.The contents of each element in Cnidii Fructus from different origins differgreatly.Conclusion： The established method is proved by methodology validation that it can be used for the determination of 16 rare earth elements in Cnidii Fructus, which provides a reference for the quality control of Cnidii Fructus.