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目的:建立同时测定注射用氟脲苷含量及有关物质的HPLC方法。方法:采用反相高效液相色谱法,色谱柱为Venusil XBP C18(4.6 mm×250 mm,5μm),以磷酸盐缓冲液(用磷酸调pH至6.6)为流动相A,流动相A-甲醇(50∶50)为流动相B,梯度洗脱:(0~20 min,95%A→60%A;20~30 min,60%A;30~35 min,60%A→95%A),流速为1.0 mL·min-1;柱温:35℃;检测波长为268 nm。结果:氟脲苷峰与各主要杂质峰均分离良好,氟脲苷浓度在63.48~571.32μg·mL-1范围内,与峰面积呈良好的线性关系,回归方程A=15.822C+13.224,r=1.000(n=7);重复性试验RSD为0.41%(n=6);平均加样回收率(n=9)为99.2%(RSD=0.48%);最低检测限为21.08 ng;供试品溶液在24 h内稳定。结论:本方法准确、灵敏,专属性强,适用于注射用氟脲苷的质量控制。
OBJECTIVE: To establish a HPLC method for the simultaneous determination of the content of fuflunin in injection and related substances. Methods: RP-HPLC was used. The mobile phase consisted of Venusil XBP C18 (4.6 mm × 250 mm, 5 μm), phosphate buffer (adjusted to pH 6.6 with phosphoric acid), mobile phase A-methanol (50:50) as mobile phase B, gradient elution: (0-20 min, 95% A → 60% A; 20-30 min, 60% A; 30-35 min, 60% A → 95% , The flow rate was 1.0 mL · min-1; the column temperature was 35 ℃; the detection wavelength was 268 nm. Results: The results showed that the peak of UF was separated well from the main impurity peaks. The concentration of UF was in the range of 63.48-557.132μg · mL-1, showing a good linear relationship with the peak area. The regression equation A = 15.822C + 13.224, r = 1.000 (n = 7); RSD of repeatability test was 0.41% (n = 6); mean recovery was 99.2% (n = 9); RSD was 0.48% The product solution is stable within 24 h. Conclusion: The method is accurate, sensitive and specific. It is suitable for the quality control of.