摘要
建立苯磺酸氨氯地平片中苯磺酸甲酯和苯磺酸乙酯超高效液相色谱质谱的检测方法.采用梯度洗脱法同时对苯磺酸甲酯和苯磺酸乙酯进行检测,流动相A为10mmol/L的乙酸铵溶液,流动相B为甲醇,色谱柱为Thermo Gold C_(18)(1.9μm,2.1 mm×50 mm),流速为0.3 mL/min,柱温为40℃,进样量为5μL.基于苯磺酸甲酯(定量离子对173.1/155.1,定性离子对173.1/91.0)和苯磺酸乙酯(定量离子对204.0/159.1)优化的质谱法,方法线性良好(苯磺酸甲酯:y=1080x+467,r=0.9998.苯磺酸乙酯:y=237x+189,r=0.9999),苯磺酸甲酯和苯磺酸乙酯的检测精密度分别为94.0和97.3%,准确度分别为101.9%和99.3%,相对标准偏差在n=12时分别为1.8%和1.4%,在n=9时分别为4.5%和4.2%,检测限均为1 ng/mL.研究表明,建立的检测方法快速、灵敏、重现性好,可用于苯磺酸氨氯地平片中苯磺酸甲酯和苯磺酸乙酯残留量的定量检测.
This paper established a UPLC-MS method for the determination of methyl and ethyl benzenesulfonate in amlodipine besylate tablets.The gradient elution was performed for the determination of methyl and ethyl benzenesulfonate through a 10 mmol/L ammonium acetate-methanol mobile phase system using a Thermo Gold C_(18)(1.9μm,2.1×50 mm)column with a flow rate of 0.3 mL/min,an injection volume of 5μL and a column temperature of 40℃.Optimized mass spectrometry based on methyl benzenesulfonate(quantitative ion pair 173.1/155.1,qualitative ion pair 173.1/91.0)and ethyl benzenesulfonate(quantitative ion pair 204.0/159.1)showed that the linearity of the method was good[y=1080x+467(r=0.9998)(methyl benzenesulfonate),y=237x+189(r=0.9999)(ethyl benzenesulfonate)].The precision of methyl benzenesulfonate and ethyl benzenesulfonate was 94.0 and 97.3%respectively,the accuracy was 101.9%and 99.3%respectively,the RSD was 1.8%and 1.4%(n=12)respectively[RSD was 4.5%and 4.2%(n=9)],and the detection limit was both 1 ng/mL.Results showed that the method was rapid,sensitive and reproducible,and can be used to quantitatively determine the residues of methyl benzenesulfonate and ethyl benzenesulfonate in amlodipine benzenesulfonate tablets.
作者
蔡志威
梁键谋
陈超
陈悦
鲍立曾
劳伦·鲁尔曼
CAI Zhiwei;LIANG Jianmou;CHEN Chao;CHEN Yue;BAO Lizeng;RUHLMANN Laurent(Zhejiang Institute for Food and Drug Control,Zhejiang Key Laboratory of Quality Control Research on Pharmaceutical Contact Materials,Hangzhou,China 310052;Zhejiang Deende Pharmaceutical Co.,Ltd.Xinchang,China 312560;Institut de Chimie,Universitéde Strasbourg,Strasbourg,France 67081)
出处
《温州大学学报（自然科学版）》
2024年第1期33-41,共9页
Journal of Wenzhou University(Natural Science Edition)
基金
国家重大科技专项药物一致性评价关键技术与标准研究(2017ZX09101001)
国家药品监督管理局仿制药评价关键技术重点实验室开放课题(GZYZF2021001)
浙江省药品监管系统科技计划项目(2023003)。
