Objective: To develop a method for the determination of three epimers in saxagliptin by high performance liquid chromatography. Methods: Chromatographic separation was carried out at 35 ℃,using Shim-pack VP-ODS（250 mm×4.6 mm,5 μm）column with mobile phases A（0.01 mol·L-1 potassium dihydrogen phosphate solution（containing 0.05 mol·L-1 sodium perchlorate））and B[acetonitrile-water-phosphoric acid （90∶10∶0.1）]. The flow rate was 1.0 mL·min-1,the injection volume was 20 μL,the detection wavelength was 210 nm. Principal component with correction factors as external standard was used to calculate the content of each epimer. The correction factors of epimer A,epimer B and epimer C were 1.07,1.07 and 1.09,respectively. Results: Saxagliptin,epimer A,epimer B and epimer C are well separated. The epimer A,epimer B and epimer C had good linear relationship in 0.245 4-2.944 5 μg·mL-1,0.252 7-3.032 2 μg·mL-1,0.234 3-2.811 0 μg·mL-1 （r was 0.999 0-1.000）,respectively. The recoveries of epimer A,epimer B and epimer C were 96.8%,98.3% and 97.4%（n=9）,respectively. The RSD of precisions were all less than 2.0%. The RSD of repeatability was 1.4%, 1.6% and 1.3%,respectively. The detection limit was 49.1,41.7 and 46.9 ng·mL-1,respectively. In the three batches of sample,the content of epimers did not exceed the detection limit（< LOD）. Conclusion: The method is simple,accurate and reproducible. It can be used for the determination of epimer A,epimer B and epimer C in saxagliptin.
DONG Xing-hua, WU Huan, ZHANG Ling-zhi, CAO Jie-yong
. Determination of three epimers in saxagliptin by high performance liquid chromatography[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(6)
: 1072
-1077
.
DOI: 10.16155/j.0254-1793.2021.06.19
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