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目的:建立白凡士林中11种微量元素的测定方法。方法:采用电感耦合等离子质谱法(ICP-MS)测定药用辅料白凡士林中Mg、Al、Fe、Co、Ni、Cu、Zn、As、Cd、Hg、Pb的含量。ICP-MS工作参数:氩气压力0.6 MPa,氦气压力0.12 MPa,扫描次数200,冲洗时间45 s,取样时间45 s,内标工作液在线加入。结果:各元素标准溶液在0~100 ng·ml~(-1)的浓度范围内,浓度与响应值的线性关系良好,除镁和铁元素相关系数分别为0.998和0.997外,其他元素相关系数均>0.999,其中,Mg、Fe、Ni、Zn、As、Pb元素的加样回收率在74.9%~83.0%之间,Cd、Hg元素的加样回收率在87.5%~94.4%之间,Al、Co、Cu元素的回收率在107.6%~118.7%,Mg、Al、Fe、Co、Ni、Cu、Zn、As、Cd、Hg、Pb检出限依次为1.9,0.59,0.61,0.16,0.33,1.5,1.7,0.09,0.12,0.70,1.6 ng·ml~(-1)。67批样品中,Mg、Al、Fe、Ni、Cu、Zn、As、Hg元素均有检出,而Co、Cd、Pb元素只在部分样品中检出。结论:本法操作简单、灵敏度高等优点,能满足微量元素的测定;建议选择含量稍高的镁、铝、铁、镍4个元素作为该品种的评价指标。
Objective: To establish a method for the determination of eleven trace elements in white petrolatum. Methods: The contents of Mg, Al, Fe, Co, Ni, Cu, Zn, As, Cd, Hg and Pb in white petrolatum were determined by inductively coupled plasma mass spectrometry (ICP-MS) ICP-MS operating parameters: argon pressure 0.6 MPa, helium pressure 0.12 MPa, scanning times 200, washing time 45 s, sampling time 45 s, the internal standard working solution was added online. Results: The calibration curve of each element standard solution was linear in the range of 0-100 ng · ml ~ (-1) with the correlation coefficients of 0.998 and 0.997 The average recoveries of Mg, Fe, Ni, Zn, As and Pb were between 74.9% and 83.0%, and the recoveries of Cd and Hg were between 87.5% and 94.4% The detection limits of Cu, Al, Co, Ni, Cu, Zn, As, Cd, Hg and Pb were in the range of 107.6% -118.7%, followed by 1.9,0.59,0.61,0.16, 0.33, 1.5, 1.7, 0.09, 0.12, 0.70 and 1.6 ng · ml -1. Among the 67 batches of samples, the elements Mg, Al, Fe, Ni, Cu, Zn, As and Hg were detected, while the elements Co, Cd and Pb were only detected in some samples. Conclusion: This method is simple, sensitive and can meet the determination of trace elements. It is suggested that four elements of magnesium, aluminum, iron and nickel with slightly higher content should be chosen as the evaluation index of this species.