电感耦合等离子体质谱法测定富马酸伏诺拉生片及其原料药中7种元素杂质含量  

Determination of Seven Elemental Impurities in Vonoprazan Fumarate Tablets and Its Raw Materials by Inductively Coupled Plasma-Mass Spectrometry

作　　者：龚翠云 朱婧 王玲兰 刘秀 彭国卿 GONG Cuiyun;ZHU Jing;WANG Linglan;LIU Xiu;PENG Guoqing(Zhuzhou Qianjin Pharmaceutical Co.,Ltd.,Zhuzhou,Hunan,China 412000)

机构地区：[1]株洲千金药业股份有限公司,湖南株洲412000

出　　处：《中国药业》2024年第14期91-94,共4页China Pharmaceuticals

基　　金：湖南省自然科学基金[2022JJ80049]。

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。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 1550 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 0-30 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(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.

关 键 词：电感耦合等离子体质谱法 富马酸伏诺拉生片 原料药 元素杂质 含量测定 

分 类 号：R917[医药卫生—药物分析学]