| 王馨远,周颖,魏宁漪.核磁共振内标法测定盐酸甲氯芬酯的含量[J].中国药品标准,2019,20(2):119-122 |
| 核磁共振内标法测定盐酸甲氯芬酯的含量 |
| Quantitative determination of Meclofenoxate Hydrochloride by proton nuclear magnetic resonance with internal standard method |
| 投稿时间：2018-10-25 修订日期：2019-04-02 |
| DOI： |
| 中文关键词: 盐酸甲氯芬酯 核磁共振 含量测定 质量平衡法 |
| 英文关键词: Meclofenoxate Hydrochloride quantitative nuclear magnetic resonance(Q-MNR) assay mass balance |
| 基金项目: |
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| 摘要点击次数: 688 |
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| 中文摘要: |
| 目的：建立1H-NMR核磁共振定量法(简称Q-NMR法)测定盐酸甲氯芬酯的含量。方法：采用Bruker AVANCE Ⅱ 400型核磁共振谱仪,以马来酸为内标,氘代水为溶剂,测定1H-NMR谱。通过样品与内标物质响应峰面积比较,测定盐酸甲氯芬酯的含量。结果：以盐酸甲氯芬酯δ6.77处峰和内标δ6.20处峰面积比值与质量比进行线性回归,线性关系良好。盐酸甲氯芬酯的质量分数为101.2%,RSD值为0.4%(n=3),重复性良好,与质量平衡法测定结果一致；验证了盐酸甲氯芬酯的成盐比例为1:1。结论：本文建立的核磁定量的方法准确、快速,为该品种的质量控制和对照品的标定提供了新的方法, 并为质量平衡法定值提供有力的佐证。 |
| 英文摘要: |
| Objective：To establish a quantitative nuclear magnetic resonance (Q-NMR) method for the determination of the absolute content of Meclofenoxate Hydrochloride. Methods：Proton nuclear magnetic resonance spectroscopy [1H-NMR] spectra were obtained in D2O with the internal standard Maleic Acid by using a Bruker AVANCE Ⅱ 400 spectrometer. The mass fraction of Meclofenoxate Hydrochloride were calculated by comparing the peak area of Meclofenoxate Hydrochloride with the internal reference substance. Results：There was a good regression between quantitative peaks ration of signals at δ6.77 of Meclofenoxate Hydrochloride and δ6.20 of internal reference substance versus mass ratio. Based on NMR, the mass fraction of Meclofenoxate Hydrochloride was 101.2% with RSD of 0.4% (n=3). It was verified meclofenoxate hydrochloride salt ratio of 1:1. Conclusion：The study provides a new way for the quality control and calibration of a reference standard material, it could be the complementary with the mass balance method for the assay of standard reference. |
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