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定量核磁共振氢谱法测定那屈肝素钙中钙离子的含量

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  • 中国食品药品检定研究院,北京 102629
第一作者 徐翊雯 Tel:(010)53852024;E-mail:xuyiwen@nifdc.org.cn
李馨白 Tel:(010)53852026;E-mail:lixinbai1105@163.com
*Tel:(010)53852026;E-mail:wuxf99@163.com

收稿日期: 2022-10-07

  网络出版日期: 2024-06-24

Determination of calcium ion content in nadroparin calcium by quantitative proton nuclear magnetic resonance spectroscopy

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  • National Institutes for Food and Drug Control, Beijing 102629, China

Received date: 2022-10-07

  Online published: 2024-06-24

摘要

目的: 建立采用定量核磁共振氢谱法(qHNMR法)测定那屈肝素钙中钙离子含量。方法: 采集核磁共振氢谱(1H NMR),zg 30脉冲,弛豫延迟时间为15 s,选择乙二胺四乙酸(EDTA)与钙离子络合物Ca-EDTA的信号峰作为钙离子的定量峰,以马来酸为内标物,对那屈肝素钙中钙离子进行定量分析。结果: Ca-EDTA和马来酸定量峰信号在1H NMR谱上分离度良好,样品与内标物的质量比在0.546~12.238,与其定量峰面积比呈线性关系(r=0.999 9),精密度RSD为0.65%,重复性RSD为0.77%,平均加样回收率为99.7%(RSD为1.3%),采用qHNMR测定9批那屈肝素钙样品中钙离子含量为9.54%~9.99%,测定结果与电感耦合等离子体发射光谱法(ICP-AES)测定结果基本一致。结论: 建立的qHNMR法操作简便、快速、准确,可用于那屈肝素钙中钙离子含量的测定。

本文引用格式

徐翊雯, 李馨白, 王瑾, 孙会敏, 吴先富 . 定量核磁共振氢谱法测定那屈肝素钙中钙离子的含量[J]. 药物分析杂志, 2023 , 43(7) : 1183 -1188 . DOI: 10.16155/j.0254-1793.2023.07.11

Abstract

Objective: To establish a quantitative proton nuclear magnetic resonance (qHNMR) spectroscopy method for the determination of calcium ion content in nadroparin calcium. Methods: Proton nuclear magnetic resonance (1H NMR) spectra, zg 30 pulses were collected, the relaxation delay time was 15 s, the signal peak of ethylenediaminetetraacetic acid (EDTA) and calcium ion complex Ca-EDTA was selected as the quantitative peak of calcium ion, maleic acid was used as the internal standard, the quantitative analysis of calcium ions in nadroparin calcium was carried out. Results: The quantitative peak signals of Ca-EDTA and maleic acid were well resolved in 1H NMR spectrum, andthe mass ratio of sample to internal standard was in the range of 0.546-12.238, the quantitative peak area ratio showed a good linear relationship (r=0.999 9), the precision RSD was 0.65%, repeatability RSD was 0.77%, the average recovery was 99.7% (RSD was 1.3%). The test results of calcium ion content in nadroparin calcium fromnine batches determined by qHNMR were 9.54%-9.99%, and the results were basically consistent with those determined by ICP-AES. Conclusion: The established qHNMR method is simple, rapid, and accurate. It can be used for the determination of calcium ion content in nadroparin calcium.

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