定量核磁共振波谱法测定坎地沙坦酯氨氯地平片中2个活性成分的绝对含量
Determination of absolute contents of candesartan cilexetil and amlodipine besylate in candesartan cilexetil and amlodipine tablets by quantitative nuclear magnetic resonance
张中玲 1吴洪海 2陈忠奎 3翁勤洁4
作者信息
- 1. 浙江大学工程师学院,杭州 310000;杭州先导医药科技有限责任公司,杭州 311100
- 2. 浙江大学药学院,杭州 310058
- 3. 杭州先导医药科技有限责任公司,杭州 311100
- 4. 浙江大学药物安全评价研究中心,杭州 310058;浙江大学台州研究院,台州 318001
- 折叠
摘要
目的:建立坎地沙坦酯氨氯地平片中坎地沙坦酯及苯磺酸氨氯地平2个活性成分绝对含量的定量核磁共振氢谱测定方法.方法:以坎地沙坦酯化学位移δ5.51,苯磺酸氨氯地平化学位移δ5.31为定量峰,马来酸化学位移δ 6.27为内标定量峰,氘代二甲基亚砜(DMSO-d6)为溶剂,使用超导核磁共振波谱仪采集供试液的氢谱,对坎地沙坦酯氨氯地平片中坎地沙坦酯及苯磺酸氨氯地平2个活性成分绝对含量进行定量测定.结果:该方法专属性强,溶剂峰、水峰及辅料峰对待测定量峰无干扰.坎地沙坦酯在1.580 0～9.480 2 mg·mL-1质量浓度范围内呈现良好的线性关系r=1.000,精密度、重复性及稳定性的RSD分别为0.070％、1.7％和0.68％,低、中、高浓度加标回收率在98.1％～99.2％;苯磺酸氨氯地平在0.983 9～5.903 6 mg·mL-1质量浓度范围内呈现良好的线性关系(r=0.999 9),精密度、重复性及稳定性的RSD分别为0.050％、1.8％和0.79％,低、中、高浓度加标回收率在99.1％～102.0％.运用该方法对2批参比制剂及不同来源的1批样品进行测试,坎地沙坦酯含量在98.10％～98.75％,苯磺酸氨氯地平含量在98.98％～99.60％.结论:该方法检测坎地沙坦酯氨氯地平片中2个活性成分的绝对含量快速、准确,且无需提供2个物质单组分对照品,为坎地沙坦酯氨氯地平片含量测定提供新的方法.
Abstract
Objective:To establish a method for determining the absolute contents of candesartan cilexetil and am-lodipine besylate in candesartan cilexetil and amlodipine tablets by qNMR Methods:The chemical shift δ 5.51 of candesartan cilexetil and δ 5.31 of amlodipine besylate were used as the quantitative peaks.δ 6.27 of maleic acid was the quantitative peak of internal standard.DMSO-d6 was used as the solvent.Results:The method was highly specific and the solvent peak,water peak and excipient peaks did not interfere with the quantitative peaks.Candesartan cilexetil showed a good linear relationship in the concentration range of 1.580 0-9.480 2 mg· mL-1,r=1.000,RSDs of precision,repeatability and stability were 0.070％,1.7％and 0.68％,respectively.The recoveries of low,medium and high concentration spiked were 98.1％-99.2％.The linear range of amlodip-ine besylate was 0.983 9-5.903 6 mg·mL-1(r=0.999 9).The RSDs of precision,repeatability and stability were 0.050％,1.8％and 0.79％,respectively.The recovery of amlodipine besylate was 99.1％-102.0％.This method was used to test two batches of reference preparations and one batch of sample from different sources.The results showed that the content of candesatan cilexetil was between 98.10％to 98.75％,and that of amlldip-ine besylate was between 98.98％to 99.60％.Conclusion:This method is rapid and accurate and it is not nec-essary to use a single component reference substance.This method provides a new method to determine the content to candesartan cilexetil and amlodipine tablets.
关键词
坎地沙坦酯/苯磺酸氨氯地平/绝对含量/定量核磁共振法Key words
candesartan cilexetil/amlodipine besilate/absolute content/quantitative nuclear magnetic resonance引用本文复制引用
出版年
2024
NETL
NSTL
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