[关键词]
[摘要]
目的 建立喜炎平注射液中17种重金属及有害元素的含量测定方法。方法 样品经消解后采用电感耦合等离子体质谱(ICP-MS)法测定,射频功率1 550 W;蠕动泵转速0.3 r/s;等离子气体积流量15 L/min;辅助气体积流量0.2 L/min;载气体积流量1 L/min;采样深度10 mm,重复次数为3次。结果 该方法下Li、Al、V、Cr、Fe、Co、Ni、Cu、As、Ag、Cd、Sn、Sb、Ba、Hg、Pb、Bi的检测限分别为9.584、49.858、0.504、3.016、51.209、0.142、1.116、0.675、0.924、1.421、0.403、2.770、0.711、3.584、0.590、0.411、0.169 ng/mL,定量限分别为28.933、151.085、1.528、9.139、155.179、0.429、3.381、2.046、2.799、4.312、1.220、8.394、2.155、10.861、1.965、1.244、0.513 ng/mL,各元素在一定质量浓度范围内,响应值与质量浓度的线性关系良好(r>0.999 1),进样精密度RSD在0.8%~3.8%(n=12),重复性RSD在0.7%~2.0%(n=6),17种元素的加样回收率在95.7%~104.8%。20批大生产样品检测结果:Ag为未检出,Li和V为检出但低于定量限,Al、Ni、Cu、As、Ba、Hg、Pb最大质量浓度分别为0.685、0.013、0.007、0.006、0.208、0.070、0.027 μg/mL,Cr、Fe、Co、Cd、Sn、Sb、Bi为未检出或检出但低于定量限。结论 方法的专属性、线性、灵敏度、精密度、准确度、耐用性等均良好,可用于喜炎平注射液中Li、Al、V、Cr、Fe、Co、Ni、Cu、As、Ag、Cd、Sn、Sb、Ba、Hg、Pb、Bi 17种元素的含量测定,20批大生产样品中17种元素检测结果均小于限度要求,符合规定。
[Key word]
[Abstract]
Objective To establish a method for the determination of 17 heavy metals and harmful elements in Xiyanping Injection (XI). Methods The samples were digested and determined by inductively coupled plasma mass spectrometry (ICP-MS). The RF power was 1 550 W; The peristaltic pump speed was 0.3 r/s; The plasma gas velocity was 15 L/min; The auxiliary gas velocity was 0.2 L/min; The carrier gas velocity was 1 L/min; The sampling depth was 10 mm and the signal was measured for three times. Results The detection limits of Li, Al, V, Cr, Fe, Co, Ni, Cu, As, Ag, Cd, Sn, Sb, Ba, Hg, Pb, Bi were 9.584, 49.858, 0.504, 3.016, 51.209, 0.142, 1.116, 0.675, 0.924, 1.421, 0.403, 2.770, 0.711, 3.584, 0.590, 0.411, 0.169 ng/mL, and the quantitative limits were 28.933, 151.085, 1.528, 9.139, 155.179, 0.429, 3.381, 2.046, 2.799, 4.312, 1.220, 8.394, 2.155, 10.861, 1.965, 1.244, and 0.513 ng/mL within a certain concentration range, respectively. The response value had a good linear relationship with the concentration (r>0.999 1); The RSDs (n=12) of the injection precision test were in the range of 0.8%-3.8%, the RSDs (n=6) of the repeatability were in the range of 0.7%-2.0%, and the average recoveries of 17 elements were in the range of 95.7%-104.8%. Detection results of 20 batches of mass production samples:Ag was not detected, Li and V were detected but lower than the quantitative limit, the maximum mass concentration of Al, Ni, Cu, As, Ba, Hg and Pb were 0.685, 0.013, 0.007, 0.006, 0.208, 0.070 and 0.027 μg/ml respectively, Cr, Fe, Co, Cd, Sn, Sb, and Bi were not detected or lower than the quantitative limit. Conclusion The specificity, linearity, sensitivity, precision, accuracy and durability of the method were all good. It can be used to determine 17 elements of Li, Al, V, Cr, Fe, Co, Ni, Cu, As, Ag, Cd, Sn, Sb, Ba, Hg, Pb and Bi in XI. The test results of 17 elements in 20 batches of mass production samples were less than the limit requirements, meeting the requirements.
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[基金项目]
国家中医药管理局中药标准化项目(ZYBZH-C-JX-41)