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

摘要

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-C18 column(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 mL/min,the column temperature at 30 ℃, the detected wavelength of 280 nm and the injection volume of 20 μL;the UPLC condition:the Syncronis C18 column(100 mm × 2. 1 mm, 1. 7 μm),the gradient elution with water(adjusting pH to 3. 0 by phosphoric acid)as the mobile phase A and acetonitrile as the mo-bile phase B,the flow rate of 0. 5 mL/min,the column temperature at 30 ℃,the detected wavelength of 280 nm and the injection vol-ume 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 ez-ceeded 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.%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Zorbaz SB－C18柱（250 mm ×4.6 mm，5μm），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1.5 mL/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 mL/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=0.9998），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。