高效液相色谱法测定注射用氟脲苷的含量及有关物质
HPLC determination of floxuridine content and its related substances in floxuridine solution for injection
分类号:
出版年·卷·期(页码):2014,34 (2):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
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。
-----英文摘要:---------------------------------------------------------------------------------------
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.
-----参考文献:---------------------------------------------------------------------------------------
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