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目的建立奥格列汀原料药中基因毒性杂质的HPLC测定方法。方法采用Zorbax SB-C18色谱柱(250 mm×4.6 mm,5μm),进样量:20μL;流动相为0.1%乙酸水-乙腈(65∶35);流速为1 m L·min~(-1);紫外检测器,检测波长为220 nm;柱温为25℃,色谱乙腈为溶剂。结果该方法专属性良好,测得苯磺酸异丙酯在4~60μg·m L-1内线性关系良好,平均回收率为98.56%(n=9,RSD=3.78%),溶液在8 h内稳定。结论该法操作简便,重复性好,结果准确可靠,可用于奥格列汀原料药中基因毒性杂质的测定。
OBJECTIVE To establish a method for the determination of genotoxic impurities in ototretinin by HPLC. Methods The chromatographic separation was performed on a Zorbax SB-C18 column (250 mm × 4.6 mm, 5 μm) with a loading volume of 20 μL and a mobile phase of 0.1% acetic acid in water (65:35) at a flow rate of 1 mL · min -1 ); UV detector, detection wavelength of 220 nm; column temperature of 25 ℃, acetonitrile as a solvent. Results The method was of good specificity. The calibration curve was linear in the range of 4 ~ 60μg · m L-1 with an average recovery of 98.56% (n = 9, RSD = 3.78%). After 8 h Internal stability. Conclusion The method is simple, reproducible, accurate and reliable, and can be used for the determination of genotoxic impurities in the drug of alogliptin.