ICP-MS法测定酒石酸长春瑞滨中有害元素及催化剂银残留

Measurement of the Residues of Harmful Elements and Silver Catalyst in Vinorelbine Tartrate by ICP-MS

目的:建立电感耦合等离子体质谱法测定酒石酸长春瑞滨中有害元素及催化剂银残留的方法。方法:用微波消解处理样品,电感耦合等离子体质谱内标法测定银、钒、铬、钴、镍、铜、砷、钼、镉、锡、锑、钡、铅、汞的含量。结果:上述14种元素的方法检出限分别为0.003、0.020、0.141、0.069、0.077、0.362、0.031、0.057、0.022、0.078、0.017、0.724、0.095、0.005 ng·m L-1,线性关系良好(r≥0.9988),回收率为86%~110%,RSD小于15%;同时,给出了此方法各元素的不确定度评定程序。结论:本方法采用在线加内标,可有效校正仪器漂移,抑制基体干扰,提高准确率,多元素测定便捷、准确、灵敏、可靠,可用于酒石酸长春瑞滨中有害元素及催化剂银残留的测定。

Objective： To establish a method for the measurement of the residues of harmful elements and silver catalyst in Vinorelbine Tartrate by inductively coupled plasma-mass spectrometry（ICP-MS）. Methods： The samples were dissolved by microwave digestion and Ag, V, Cr, Co, Ni, Cu, As, Mo, Cd, Sn, Sb, Ba, Pb, Hg were determined by ICP-MS with internal standard method. Results： The detection limit of the above mentioned 14 elements was 0.003, 0.020, 0.141, 0.069, 0.077, 0.362, 0.031, 0.057, 0.022, 0.078, 0.017, 0.724, 0.095, 0.005 ng·m L^-1, respectively. The results of the 14 elements showed good linearity（r≥0.9988）. The recovery rates were 86% to 110% and the relative standard deviations（RSDs） were less than 15%. Furthermore, an evaluation program for uncertainty assessment was put forward. Conclusion： The method which uses online internal standard can effectively correct instrument drift, suppress matrix interference and improve accuracy, which is convenient, accurate, sensitive and reliable and can be used to measure the residue of harmful elements and silver catalyst in Vinorelbine Tartrate.