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[摘要]
目的 建立达格列净原料药中有关物质的测定方法。方法 采用 HPLC法。Diamonsil C18色谱柱(250 mm×4.6 mm,5 μm);以0.02 mol/L磷酸二氢钠水溶液–甲醇–四氢呋喃(60:35:5)为流动相;体积流量1.0 mL/min;检测波长220 nm;柱温35 ℃;进样量为10 μL。结果 达格列净与各杂质的分离度良好,杂质Z1、Z2、F1、F2、F3的定量限分别为3.22、3.83、3.65、4.33、4.92 ng,平均回收率分别为98.9%、97.6%、103.2%、102.4%、102.8%,RSD值分别为1.8%、1.3%、1.5%、0.7%、1.7%。结论 本方法检测灵敏度高,精密度好,可以用于达格列净原料药中有关物质的质量控制。
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[Abstract]
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.
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