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

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。

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(A_s) and internal standard(A_r). Results: Each sample solution was characterized for six times and RSD of A_s/A_r was 0.99%;when spectrum was integrated for five times,RSD of A_s/A_r 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.

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