首页|超高效液相色谱质谱法同时测定苯磺酸氨氯地平片中的苯磺酸甲酯和苯磺酸乙酯

超高效液相色谱质谱法同时测定苯磺酸氨氯地平片中的苯磺酸甲酯和苯磺酸乙酯

扫码查看
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10 mmol/L的乙酸铵溶液,流动相B为甲醇,色谱柱为Thermo Gold C18(1.9 μm,2.1 mm × 50 mm),流速为0.3 mL/min,柱温为40℃,进样量为5 μL.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=1 080x+467,r=0.999 8.苯磺酸乙酯:y=237x+189,r=0.999 9),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.
Determination of Methyl Benzenesulfonate and Ethyl Benzenesulfonate in Amlodipine Besylate Tablets by UPLC-MS
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 C18(1.9 μm,2.1 × 50 mm)column with a flow rate of 0.3 mL/min,an injection volume of 5 μL 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=1 080x+467(r=0.999 8)(methyl benzenesulfonate),y=23 7x+189(r=0.999 9)(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.

Amlodipine Besylate TabletsMethyl BenzenesulfonateEthyl BenzenesulfonateUPLC-MS

蔡志威、梁键谋、陈超、陈悦、鲍立曾、劳伦·鲁尔曼

展开 >

浙江省食品药品检验研究院浙江省药品接触材料质量控制研究重点实验室,浙江杭州 310052

斯特拉斯堡大学化学研究所,法国斯特拉斯堡67081

浙江得恩德制药股份有限公司,浙江新昌 312560

苯磺酸氨氯地平片 苯磺酸甲酯 苯磺酸乙酯 液相色谱质谱法

国家重大科技专项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浙江省药品监管系统科技计划项目

2017ZX09101001GZYZF20210012023003

2024

温州大学学报(自然科学版)
温州大学

温州大学学报(自然科学版)

影响因子:0.184
ISSN:1674-3563
年,卷(期):2024.45(1)
  • 14