HPLC测定苯甲酸阿格列汀片中对映异构体的含量

金朱雨; 谢升谷; 黄巧巧

doi:10.13748/j.cnki.issn1007-7693.20242033

HPLC测定苯甲酸阿格列汀片中对映异构体的含量

Determination of Enantiomer Content in Alogliptin Benzoate Tablets by HPLC

摘要

摘要:
目的建立分离阿格列汀及其对映异构体的HPLC，并对苯甲酸阿格列汀片中对映异构体的含量进行测定。
方法使用以硅胶表面涂敷直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)为填充剂的色谱柱Daicel CHIRALPAK AD-H(4.6 mm×250 mm，5 μm)，检测波长为278 nm，柱温为40 ℃，流速为1.0 mL·min⁻¹，流动相为正己烷-无水乙醇-甲烷磺酸(80∶20∶0.3)，进样体积为20 μL。
结果苯甲酸阿格列汀片中对映异构体在优化的手性分离条件下能够被完全分离；出峰顺序为对映异构体峰在前，阿格列汀峰在后；浓度在0.02~2.0 μg·mL⁻¹内，阿格列汀对映异构体的浓度与峰面积呈现良好的线性关系；阿格列汀对映异构体的加标回收率为98.90%~101.24%，相对标准偏差为0.97%，表明该方法准确度良好。
结论建立的方法简便、准确、灵敏度高，可用于苯甲酸阿格列汀片中对映异构体的分离及含量测定。

Abstract:
OBJECTIVE To establish an HPLC method for the separation of alogliptin and its enantiomer, and to determine the content of the enantiomer in alogliptin benzoate tablets.
METHODS A chiral column packed with amylose tris(3,5-dimethylphenylcarbamate) coated on silica gel, Daicel CHIRALPAK AD-H(4.6 mm×250 mm, 5 μm), was used. The detection wavelength was 278 nm; the column temperature was 40 °C; the flow rate was 1.0 mL·min⁻¹; the mobile phase consisted of n-hexane, anhydrous ethanol, methanesulfonic acid in the ratio of 80∶20∶0.3; the injection volume was 20 μL.
RESULTS Under the optimized chiral separation conditions, alogliptin benzoate and its enantiomer were completely separated, with the enantiomer peak appearing before the alogliptin peak. A good linear relationship was observed between the concentration of alogliptin enantiomer and the peak area in the range of 0.02 to 2.0 μg·mL⁻¹. The recovery rates of spiked alogliptin enantiomer were between 98.90%−101.24%, with relative standard deviations of 0.97%, indicating good accuracy of the method.
CONCLUSION The established method is simple, accurate, and sensitive, and can be used for the separation and quantification of alogliptin benzoate and its enantiomer.

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