摘要
目的:建立同时测定甲磺酸酚妥拉明注射液中9种元素含量的电感耦合等离子体质谱法(ICP-MS),以评估迁移风险。方法:以钪(Sc)和铑(Rh)为目标,建立ICP-MS法同时测定锑(Sb)、镉(Cd)、铅(Pb)、砷(As)、硅(Si)、硼(B)、钡(Ba)、钾(K)和铝(Al)含量。测定模式为KDE模式,射频功率为1548.6 W,等离子体气流量为13.783 L·min^(-1),载气流量为1.04 L·min^(-1),辅助气流量为0.78 L·min^(-1)。结果:元素As、Cd、Sb、Pb在0 ng·mL^(-1)~100 ng·mL^(-1),元素B、Al、Si、K、Ba在0 ng·mL^(-1)~1000 ng·mL^(-1)线性范围内,具有良好的线性关系(r≥0.998)。9种元素平均回收率分别为104.47%(Sb)、101.19%(Cd)、96.52%(Pb)、88.78%(As)、100.46%(Si)、95.81%(B)、102.96%(Ba)、101.79%(K)和102.38%(Al),回收率均在80%~120%。结论:ICP-MS法操作简单、快速,验证试验结果表明,此方法专属性强,灵敏度高,可以用于甲磺酸酚妥拉明注射液中9种元素的测定,为评估甲磺酸酚妥拉明注射液中元素迁移风险提供技术支持,为更合理地控制药品质量提高。
Objective:To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for simultaneous determination of nine elements in phentolamine mesilate injection to evaluate migration risk.Method:The ICP-MS method was established to simultaneously determine the element contents of Sb,Cd,Pb,As,Si,B,Ba,K and Al using Sc and Rh internal standards.The measurement mode is KDE mode,the RF power is 1548.6 W,the plasma gas flow rate is 13.783 L·min^(-1),the carrier gas flow rate is 1.04 L·min^(-1) and the auxiliary gas flow rate is 0.78 L·min^(-1).Result:As、Cd、Sb and Pb have a good linear relationship within the range of 0 ng·mL^(-1) to 100 ng·mL^(-1),while B、Al、Si、K and Ba have a linear relationship within the range of 0 ng·mL^(-1) to 1000 ng·mL^(-1)(r≥0.998).The average recovery rates of 9 elements are 104.47%(Sb)、101.19%(Cd)、96.52%(Pb)、88.78%(As)、100.46%(Si)、95.81%(B)、102.96%(Ba)、101.79%(K)and 102.38%(Al),with recovery rates ranging from 80%to 120%.Conclusion The ICP-MS method is simple and fast to operate.The validation test results show this method has strong specificity and high sensitivity,and the method can be used for the determination of 9 elements in phentolamine mesilate injection.It provides technical support for evaluating the migration risk of elements in phentolamine mesilate injection and improving the quality control of drugs more reasonably.
作者
陈鸿玉
王晓菲
王皖
李钰鑫
李帅
郑金凤
李琦
盛忻
Chen Hongyu;Wang Xiaofei;Wang Wan;Li Yuxin;Li Shuai;Zheng Jinfeng;Li Qi;Sheng Xin(Hunan Institute for Drug Control,Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Key Laboratory of Pharmaceutical Excipient Engineering Technology of State Drug Administration,Changsha 410001,China)
出处
《广东化工》
2025年第12期147-149,113,共4页
Guangdong Chemical Industry
基金
2023年国家药品抽检(国药监药管[2023]2号)。
关键词
甲磺酸酚妥拉明
电感耦合等离子体质谱法
元素测定
迁移量
风险评估
phentolamine mesilate
inductively coupled plasma mass spectrometry
elemental determination
migration amount
risk assessment
