超高效及高效液相色谱法测定华法林钠片含量的结果比对

Comparison of Results of Content Determination of Warfarin Sodium Tablets by UPLC and HPLC

目的建立测定华法林钠片含量的超高效液相色谱（UPLC）法,并与高效液相色谱（HPLC）法测定结果进行比对。方法 HPLC法条件为Zorbax SB-C18柱（250 mm×4.6 mm,5μm）,以水（用磷酸调p H至3.0）为流动相A、乙腈为流动相B进行梯度洗脱,流速为1.5 m L/min,柱温为30℃,检测波长为280 nm,进样量为20μL;UPLC法条件为Syncronis C18柱（100 mm×2.1 mm,1.7μm）,以水（用磷酸调pH至3.0）为流动相A、乙腈为流动相B进行梯度洗脱,流速为0.5 m L/min,柱温为30℃,检测波长为280 nm,进样量为5μL。结果建立的UPLC法测定华法林钠片含量方法中,华法林钠进样量在0.284~0.758μg范围内与峰面积呈良好线性关系（r=0.999 8）,平均回收率为99.45%,RSD=0.53%（n=9）,系统适用性试验远超标准要求。结论该方法快速灵敏、准确可靠、重复性好,可用于华法林钠片的含量测定。

Objective To establish a method for the content determination of Warfarin Sodium Tablet by the ultra performance liquid chromatography（ UPLC） and to conduct the comparison with the high performance liquid chromatography（ HPLC）. Methods The HPLC condition： the ZORBAX SB- C18column（ 250 mm × 4. 6 mm,5 μm）,the gradient elution with water（ adjusting pH to 3. 0 by phosphoric acid） as the mobile phase A and acetonitrile as the mobile phase B,the flow rate of 1. 5 m L / min,the column temperature at 30 ℃,the detected wavelength of 280 nm and the injection volume of 20 μL; the UPLC condition： the Syncronis C18column（ 100 mm × 2. 1 mm,1. 7 μm）,the gradient elution with water（ adjusting p H to 3. 0 by phosphoric acid） as the mobile phase A and acetonitrile as the mobile phase B,the flow rate of 0. 5 m L / min,the column temperature at 30 ℃,the detected wavelength of 280 nm and the injection volume of 5 μL. Results In the established method of the content determination of Warfarin Sodium Tablets by UPLC,the linear range was 0. 284- 0. 758 μg（ r = 0. 999 8）. The average recovery was 99. 45%,RSD = 0. 53%（ n = 9）. The system suitability test greatly exceeded the standard requirements. Conclusion The method is rapid,sensitive and accurate with good reproducibility,which can be used for the content determination of Warfarin Sodium Tablet.