高效液相色谱法测定注射用氟脲苷的含量及有关物质

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，5 μm），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63.48~571.32 μg·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 an HPLC method to determine the floxuridine content and its related substances in the floxuridine solution for injection. Methods: The analysis was achieved on a Venusil XBP C₁₈ column (250 mm×4.6mm,5 μm) using a mobile phase of methonal-phosphoric acid buffer(pH adjusted to 6.6 with phosphoric acid) with gradient elution in a total runing time of 35 min(0-20 min,95% A→60% A;20-30 min,60% A;30-35 min,60% A→95% A).The flow rate was 1.0 mL·min^-1 and the column temperature was 35 ℃ and the detection wave length was 268 nm. Results: There was a good resolution among the peaks of floxuridine and the main related substances.There was a good linear relationship between the peak area and the concentration of floxuridine in the range of 63.48-571.32 μg· mL^-1 (r=1.000,n=7).Regression equation could be expressed by A=15.822C+13.224.The average recovery was 99.2%(RSD=0.48%,n=9),the RSD of the repeatability test was 0.41% (n=9),and the limit of detection was 21.08 ng.The solution was stable for 24 hours. Conclusions: The method is specific,accurate and sensitive,which can be used for quality control of the floxuridine solution for injection.

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