¹H与¹³C核磁共振定量技术在聚桂醇成分分析中的应用比较

目的：建立¹³C核磁共振定量（qNMR）测定聚桂醇中脂肪碳链长度及聚氧乙烯醚的聚合度的方法，比较¹³C qNMR和¹H qNMR测定方法之间的异同。方法：在¹³C qNMR试验中，以乙酰丙酮铬（Ⅲ）为弛豫试剂，氘代氯仿甲醇为混合溶剂，采用反门控去偶的zgig30脉冲序列测定聚桂醇成分；在¹H qNMR试验中，以氘代氯仿为溶剂，采用zg30脉冲序列测定聚桂醇成分。结果：通过¹³C qNMR技术测得聚桂醇样品中脂肪碳链长度为13.6，聚氧乙烯醚的聚合度n=9.4，与使用¹H qNMR技术测定的结果（脂肪碳链长度为12.4，聚氧乙烯醚的聚合度n=9.4）相近。结论：¹³C qNMR与¹H qNMR均能准确测定聚桂醇成分，¹H qNMR技术使用样品量少，检测速度快，但响应信号重叠多，精确度低，适用于快检初筛；¹³C qNMR技术需要样品量大，耗时长，抗干扰能力强，适合进一步精确测定聚桂醇成分。

Objective: To establish a ¹³C quantitative nuclear magnetic resonance (qNMR) method in analysis of the average chain length of the fatty alcohol and the average number of moles of polyethylene oxide in lauromacrogol,and to compare the difference between ¹H qNMR and ¹³C qNMR methods.Methods: In ¹³C qNMR experiment,chromium (Ⅲ) acetylacetonate was used as a relaxation reagent,CDCl3 and deuterated methanol mixture was used as solvent,and zgig30 pulse sequence was deployed;In ¹H qNMR experiment,CDCl3 was used as solvent and zg30 pulse sequence was applied.Results: Based on ¹³C qNMR experiments,the average chain length of the fatty alcohol was 13.6 and the average number of moles of polyethylene oxide was 9.4.Both results were similar to those obtained from ¹H qNMR(the average chain length of the fatty alcohol was 12.4 and the average number of moles of polyethylene oxide was 9.4).Conclusion: Both ¹H and ¹³C qNMR can effectively acquire the component information of lauromacrogol.Compared with ¹³C qNMR,¹H qNMR method requires smaller amount of samples,the testing speed is quicker but with lower precision.Thus ¹H qNMR is suitable for rapid screening while ¹³C qNMR technique is a perfect tool for accurate determination of the component of lauromacrogol.

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