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5-氟胞嘧啶是一种抗真菌药,目前只能制成胶囊剂,美国药典1990版采用 UV 法在波长285nm 处测其含量,其代谢产物氟尿嘧啶干扰其测定,其他的方法较繁琐且昂贵,本文报告建立一种不需要反离子的稳定的、常温下进行测定的 HPLC 法。色谱柱为 Med.Pharme×C_(18)柱(25cm×4.6mm,id),流动相为0.05mol/LKH_2PO_4缓冲液(pH 4.5),流速1.0ml/min,检测波长300nm,纸速30.5cm/h,室温。溶液配制:5-氟胞嘧啶和5-氟尿嘧啶各100.0mg 溶于足量水中,制得100.0ml 储备液,取5-氨基尿嘧啶20mg 溶于水中制成500ml 内标液。储备液和内标液需每天配制,按需要稀释。测定及计算:精称10个胶囊,取标示量为100mg 5-氟胞嘧啶的粉末混于80ml 水中,振荡3～4min,加水至100.0ml,过滤,弃去前20ml 滤液,收集续滤液备用。取续滤液2.5ml 与7.5ml 5-氨基尿嘧啶混合,加水至25.0ml。取25μl 进样分析。加入已知量标准液作比较,待测药物与内标峰高比为(R_(ph))_α,标准品与内标峰高比为(R_(ph)_s,则样
5 - fluorocytosine is an antifungal agent, currently only capsules, the United States Pharmacopoeia 1990 edition using the UV method at a wavelength of 285nm at its content, its metabolites fluorouracil interfere with its determination, the other more cumbersome and expensive , This report reports the establishment of a stable, non-ion-dependent, HPLC method for determination at ambient temperature. The chromatographic column was Med.Pharme × C_ (18) column (25cm × 4.6mm, id). The mobile phase consisted of 0.05mol / L KH_2PO_4 buffer (pH 4.5), the flow rate was 1.0ml / min, the detection wavelength was 300nm, the paper speed was 30.5cm / h, room temperature. Solution preparation: 5-fluorocytosine and 5-fluorouracil each 100.0mg dissolved in sufficient water to prepare 100.0ml stock solution, take 5-aminouracil 20mg dissolved in water to make 500ml internal standard solution. Stock solution and internal standard solution should be prepared daily and diluted as needed. Measurement and calculation: 10 capsules were accurately weighed, and the labeled amount of 5-fluorocytosine powder was mixed in 80 ml of water, shaken for 3 to 4 minutes, added with water to 100.0 ml, filtered and the filtrate of the first 20 ml was discarded to collect the filtrate. Take the filtrate 2.5ml and 7.5ml 5-aminouracil mixed, add water to 25.0ml. Take 25μl injection analysis. Add a known amount of standard solution for comparison, the peak height ratio of the drug to the internal standard (R_ (ph)) _ α, standard and internal standard peak height ratio (R_ (ph) _s, the sample