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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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19F qNMR在含氟制剂含量测定中的应用

Application of 19F qNMR in the assay of fluorine-containing preparation

作者(英文):
分类号:R917
出版年·卷·期(页码):2018,38 (9):1507-1510
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立19F核磁共振定量(qNMR)测定片剂中含氟药物含量的方法。方法:以4,4'-二氟二苯甲酮为内标,氘代DMSO为溶剂,采用反门控去耦的zgfhigqn.2脉冲序列,利用19F qNMR测定卡格列净片中卡格列净含量。试验参数如下:谱宽SW=40×10-6,射频中心频率O1P=-110×10-6,采样点数TD=128 k,采样时间AQ=3.5 s,弛豫延迟时间D1=20 s,扫描次数32次。结果:通过简单的过滤或离心处理后,使用19FqNMR测得6片卡格列净片中卡格列净含量分别为98.2%、98.9%、101.0%、99.7%、99.2%,与HPLC外标法测定结果相近。结论:19F qNMR可以用于含氟药物制剂中药品含量测定,这种技术前处理简单,检测速度快,不受辅料等干扰,可以用于含氟药物制剂含量的高通量测定。

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

Objective: To establish a 19F quantitative nuclear magnetic resonance (qNMR) method to determine the content of active pharmaceutical ingredient (API) in fluorine-containing preparation. Methods: In 19F qNMR experiments, 4, 4-difluorobenzophenone was used as an internal standard. DMSO-d6 was used as solvent and zgfhigqn.2 pulse sequence with inverse gated decoupling was applied. Other parameters were as follows:SW=40×10-6, O1P=-110×10-6, TD=128 k, AQ=3.5 s, D1=20 s and NS=32. Results: After simple pre-treatment of filtration or centrifuge, the content of canagliflozin in 5 tablets were measured using 19F-qNMR. The results were 98.2%, 98.9%, 101.0%, 99.7% and 99.2%, respectively. The results were similar to those from HPLC method. Conclusion: 19F qNMR can be used in determining the contents of fluorine-containing APIs in tablets. This method only requires minimal pre-treatment and its testing speed is rapid. Meanwhile, the excipients have no interference with the determination. This technology is suitable for high-throughput measuring the API content in fluorine-containing preparation.

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