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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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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

Comparison of 1H and 13C quantitative nuclear magnetic resonance in component analysis of lauromacrogol

作者(英文):
分类号:R917
出版年·卷·期(页码):2018,38 (4):716-719
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

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: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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------
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