1-乙酰基-3-邻甲基苯甲酰基-5-氟尿嘧啶含量及其杂质的高效液相色谱测定

Assay and Determination of Impurity for 1 - Acetyl -3-o -Toluyl- 5 - Fluorouracil and Its Preparation by HPLC

目的:采用高效液相色谱法测定1-乙酰基-3-邻甲基苯甲酸基-5-氟尿嘧啶的含量及其有关物质。方法:以菲为内标物质,采用氰基柱(4.6mm×200mm,Nucleosil填料,粒度5μm),以5％冰醋酸乙腈溶液-0.5％醋酸铰溶液(60:40)为流动相,流速为1mL·min^(-1) ,紫外检测器在254nm处测定。结果:线性范围为0.2～1μg,r=0.999 9;平均回收率为99.9％;供试品溶液在2h内稳定;日内和日间测定的RSD分别为0.8％(n=6)和1.1％(n=5);杂质检出限为0.08ng。结论:采用高效液相色谱法测定1-乙酰基-3-邻甲基苯甲酰基-5-氟尿嘧啶的含量及其有关物质,方法简便准确,结果可靠。

Objective: A HPLC method for determination of 1 - acetyl - 3 - o - toluyl - 5 - fluorouracil (A - OT -Fu) and its impurity 3-o - toluyl -5 -fluorouracil (TFu) was developed. Method: International standard substance; phenantherene; Column; A 4. 6 mm × 200 mm stainless steel column filled with Nucleosil CN; Mo-bile phase; 5% glacial acetic acid in acetonitrile -0. 5% ammonium acetate in water (60:40) ; Flow rate; 1 mL · min-1 ; Detective wavelength; 254 nm. Results: The linear range of assay was 0. 2 - 1 μg (r =0. 999 9) ; The average recovery of A - OT - Fu was 99. 9% . The testing solution for assay was stable within 2 hours. The RSD of the determinations for single and repetitious were respectively 0. 8% (n =6) and 1.1% ( re = 5). The least detective limit of impurity was 0. 08 ng. Conclusion: The method established is rapid, accurate and relia-ble.