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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核磁共振定量技术测定酒石酸吉米格列汀倍半水合物含量

Quantitative analysis of gemigliptin tartrate sesquihydrate by 19F quantitative NMR (19F-qNMR)

分类号:
出版年·卷·期(页码):2014,34 (7):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立19F核磁共振定量法测定酒石酸吉米格列汀倍半水合物含量。 方法:以4-溴-2-氟乙酰苯胺为内标,氘代DMSO为溶剂测定19F核磁共振谱,通过比较吉米格列汀样品定量峰与内标物质响应峰面积,计算酒石酸吉米格列汀倍半水合物的含量。 结果:同一样品在相同条件下测定6次,定量峰与内标响应峰比值的RSD为0.99%;将图谱重复积分5次,定量峰与内标峰比值的RSD为0.39%;平行配制5份样品溶液,依据定量峰与内标响应峰比值计算的酒石酸吉米格列汀倍半水合物平均含量为99.3%,RSD为0.54%,19F核磁共振定量结果与质量平衡法测定结果99.0%一致。 结论19F核磁共振定量法内标选择广泛,图谱解析简单,可以准确快速地测定酒石酸吉米格列汀倍半水合物。

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

Objective: To establish a 19F-qNMR method for the determination of gemigliptin tartrate sesquihydrate. Methods: To characterize gemigliptin tartrate sesquihydrate,a19F-NMR method was performed using4'-bromo-2'-fluoroacetanilide as an internal standard and DMSO-d6 as solvent.The gemigliptin tartrate sesquihydrate content was calculated by comparing the response peak area of sample(As) and internal standard(Ar). Results: Each sample solution was characterized for six times and RSD of As/Ar was 0.99%;when spectrum was integrated for five times,RSD of As/Ar was 0.39%;when five samples were prepared and characterized,the average content of gemigliptin tartrate sesquihydrate was 99.3% and RSD was 0.54%.The results from 19F-qNMR assay were consistent with the results from mass balance method (99.0%). Conclusion: A variety of internal standards can be used in19 F-qNMR,and their spectrums are easy to characterize.The established 19 F-qNMR method is precise and rapid for determination of gemigliptin tartrate sesquihydrate.

-----参考文献:---------------------------------------------------------------------------------------
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[3] ZHANG Qi(张琪),LI Xiao-dong (李晓东),YANG Hua-xin(杨化新).Application of nuclear magnetic resonance in pharmaceutical standards(核磁共振技术在药品标准领域中的应用进展)[J]. Chin J Pharm Anal (药物分析杂志),2012,32(3):545
[4] Dolbier WR.Guide to Fluorine NMR for Organic Chemists[M].New Jersey,USA:John Wiley & Sons,Inc.,2009:4
[5] YANG Bai-qin(杨百勤),KONG Er-li(孔二丽),XUE Xiao-di(薛潇迪),et al.Qualitative and quantitative analysis of fluoxetin hydrochloride by 19F NMR(采用核磁共振氟谱定性与定量分析盐酸氟西汀)[J].Acta Pharm Sin(药学学报),2012,47(5):630
[6] WU Yong-lan(吴永兰),WEN Qian(文茜),YANG Ming-sheng(杨明生),et al.Measurement with quantitative determination of fluoride in pazufloxacin mesilate sample by 19F nuclear magnetic resonance(氟核磁共振法定量测定甲磺酸帕珠沙星含量)[J].J Xiangnan Univ(湘南学院学报),2007,28(5):53
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