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目的建立RP-HPLC法测定苯甲酸阿格列汀原料药的含量及有关物质。方法采用Thermo ODS-2 HYPERSIL色谱柱(250 mm×4.6 mm,5μm),以乙腈-体积分数为0.1%甲酸水溶液(用三乙胺调p H值为3.0)为流动相,流速为1.0 m L·min-1,检测波长为278 nm,柱温为30℃。结果在含量测定色谱条件下,阿格列汀在质量浓度8~80 mg·L-1内与峰面积呈良好线性关系(r=0.999 8,n=5),平均回收率为99.9%(n=9);在有关物质测定色谱条件下,有关物质A、B、C、D和E在质量浓度0.1~2.0 mg·L-1内与峰面积呈良好的线性关系(r在0.999 6~0.999 8内,n=6);有关物质A、B、D和E含量均小于0.25‰,有关物质C含量小于0.4‰。结论该方法准确、专属性强,为苯甲酸阿格列汀原料药的质量控制提供了依据。
OBJECTIVE To establish a RP-HPLC method for the determination of alogliptin benzoate and its related substances. Methods The mobile phase was Thermo ODS-2 HYPERSIL column (250 mm × 4.6 mm, 5 μm) with acetonitrile-0.1% formic acid aqueous solution (p H value was 3.0 with triethylamine) as mobile phase at a flow rate of 1.0 mL Min-1, the detection wavelength was 278 nm and the column temperature was 30 ℃. Results The content of alogliptin showed a good linear relationship with the peak area (r = 0.999 8, n = 5) at the concentration of 8 ~ 80 mg · L-1 and the average recovery was 99.9% (n = 9). Under the chromatographic conditions, the related substances A, B, C, D and E showed a good linear relationship with the peak area in the range of 0.1-2.0 mg · L-1 (r = 0.999 6-0.999 8, n = 6). The contents of related substances A, B, D and E were less than 0.25 ‰ and the content of related substances C was less than 0.4 ‰. Conclusion The method is accurate and specific, which provides the basis for the quality control of alogliptin benzoate.