目的 建立達格列凈原料藥中有關物質(zhì)的測定方法。方法 采用 HPLC法。Diamonsil C₁₈色譜柱(250 mm×4.6 mm,5 μm);以0.02 mol/L磷酸二氫鈉水溶液–甲醇–四氫呋喃(60:35:5)為流動相;體積流量1.0 mL/min;檢測波長220 nm;柱溫35 ℃;進樣量為10 μL。結果 達格列凈與各雜質(zhì)的分離度良好,雜質(zhì)Z1、Z2、F1、F2、F3的定量限分別為3.22、3.83、3.65、4.33、4.92 ng,平均回收率分別為98.9%、97.6%、103.2%、102.4%、102.8%,RSD值分別為1.8%、1.3%、1.5%、0.7%、1.7%。結論 本方法檢測靈敏度高,精密度好,可以用于達格列凈原料藥中有關物質(zhì)的質(zhì)量控制。

Objective To establish a method for determination of related substances in dapagliflozin active pharmaceutical ingredients. Methods HPLC method was adopted. The determination was carried out on Diamonsil C₁₈ column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of 0.02 mol/L sodium dihydrogen phosphate-methanol-tetrahydrofuran (60:35:5) at a flow rate of 1.0 mL/min. The detective wavelength was set at 220 nm, the column temperature was at 35 ℃, and the injection volume was 10 μL. Results Dapagliflozin and its related substances had good separation. The LOQ of the related substances, such as Z1, Z2, F1, F2, and F3 were1.34, 1.54, 1.42, 1.71, and 2.11 ng, respectively. The average recoveries were 98.9%, 97.6%, 103.2%, 102.4%, and 102.8% with RSD values of 1.8%, 1.3%, 1.5%, 0.7%, and 1.7%, respectively. Conclusion The method is sensitive and accurate, and can be used for quality control of related substances in dapagliflozin active pharmaceutical ingredients.