摘要
目的 建立测定富马酸伏诺拉生片及其原料药中 7 种元素杂质含量的电感耦合等离子体质谱法(ICP-MS)法.方法 等离子功率为 1 550 W,等离子体气为氩气,流速为 14 L/min,载气为氩气,流速为 4.9 mL/min,蠕动泵转速为 40 r/min,采用动能歧视(KED)测定模式,全定量分析获取模式.结果 砷、镉、汞、铅、钴、镍、钒质量浓度分别在 0～30 ng/mL、0～12 ng/mL、0～60 ng/mL、0～12 ng/mL、0～120 ng/mL、0～120 ng/mL、0～120 ng/mL范围内与仪器响应值线性关系良好(r>0.990),检测限为 0.002～0.052 ng/mL,定量限为 0.006～0.159 ng/mL;精密度、重复性试验结果的 RSD 均小于 10.0%;平均加样回收率为 97.46%～102.11%,RSD为0.49%～4.11%(n=9).3批成品中仅检出镉、汞、铅、镍,含量分别为0.05 mg/kg、0.24～0.35 mg/kg、0.04～0.16 mg/kg、0.41～0.49 mg/kg;3批原料药中仅检出汞、镍、钒,含量分别为 0.09～0.64 mg/kg、0.28～0.38 mg/kg、0.01～0.03 mg/kg.结论 所建立的方法简单、快速,灵敏度、准确度高,精密度好,可用于富马酸伏诺拉生片及其原料药中元素杂质含量控制.
Abstract
Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the determination of seven elemental impurities in Vonoprazan Fumarate Tablets and its raw materials.Methods The plasma power was 1 550 W,the plasma gas was argon with a flow rate of 14 L/min,the carrier gas was argon with a flow rate of 4.9 mL/min,the rotation rate of peristaltic pump was 40 r/min,the kinetic energy discrimination(KED)determination mode and full-quantitative analysis acquisition mode were adopted.Results The linear ranges of arsenic,cadmium,mercury,lead,cobalt,nickel,and vanadium were 0-30ng/mL,0-12ng/mL,0-60ng/mL,0-12ng/mL,0-120ng/mL,0-120ng/mL,0-120ng/mL(r>0.990).The limit of detection(LOD)was in the range of 0.002-0.052 ng/mL,the limit of quantification(LOQ)was in the range of 0.006-0.159 ng/mL.The RSDs of precision and repeatability tests were lower than 10.0% .The average recovery rate of the above elements was in the range of 97.46%-102.11% with the RSD of 0.49%-4.11% (n=9).Only cadmium,mercury,lead,and nickel were detected in three batches of finished products,with contents of 0.05 mg/kg,0.24-0.35 mg/kg,0.04-0.16 mg/kg,and 0.41-0.49 mg/kg,respectively.Only mercury,nickel,and vanadium were detected in three batches of raw materials,with contents of 0.09-0.64 mg/kg,0.28-0.38 mg/kg,and 0.01-0.03 mg/kg,respectively.Conclusion The established method is simple,fast,sensitive,accurate,and precise,which can be used for content control of the elemental impurities in Vonoprazan Fumarate Tablets and raw materials.
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