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目的:建立恩格列净原料药纯度及所含杂质的测定方法。方法:采用高效液相色谱(HPLC)法,用Waters symmetry C18色谱柱(250 mm×4.6 mm,5μm),以0.01%(V/V)三氟乙酸溶液为流动相A,乙腈为流动相B,线性梯度洗脱:0~10 min,流动相B 32%;10~50 min,流动相B 32%~95%;检测波长225 nm,流速1.0 m L/min,柱温45℃。结果:恩格列净与各杂质的分离度均>1.5,检出限均<9 ng/m L,线性范围满足定量分析要求;重复性试验相对标准差(RSD)均<5%;供试品溶液和对照溶液在8 h内稳定性良好;各杂质的回收率为88.6%~106.1%,RSD均<10%。结论:本研究建立的方法检测灵敏度高,精密度好,可作为恩格列净原料药有关物质的控制方法。
OBJECTIVE: To establish a method for the determination of the purity and impurity of englustipha. Methods: The mobile phase A was acetonitrile-mobile phase with high performance liquid chromatography (HPLC) on a Waters symmetry C18 column (250 mm × 4.6 mm, 5 μm) using 0.01% , Linear gradient elution: 0 ~ 10 min, mobile phase B 32%; 10 ~ 50 min, mobile phase B 32% ~ 95%; detection wavelength 225 nm, flow rate 1.0 m L / min, column temperature 45 ℃. Results: The results showed that the separation of enflulocine and each impurity were all> 1.5, the detection limits were all <9 ng / m L, and the linear range satisfied the requirements of quantitative analysis. The relative standard deviations (RSDs) of repeatability tests were all less than 5% The stability of the product solution and the control solution within 8 h was good. The recoveries of all impurities ranged from 88.6% to 106.1% with RSD <10%. Conclusion: The method developed in this study has high detection sensitivity and good precision, which can be used as the control method of the related substances of the drug of the enzapine.