Meshram D B, Bagade S B, Tajne M R
Department of Pharmaceutical Sciences, RTM Nagpur University, Nagpur-440033, India.
J Chromatogr Sci. 2009 Nov-Dec;47(10):885-8. doi: 10.1093/chromsci/47.10.885.
A rapid and sensitive reversed-phase high-performance liquid chromatographic method is developed for simultaneous estimation of fluconazole, an orally active triazole anti-fungal agent, and tinidazole, which belongs to the group of 5-nitroimidazoles in combined dose tablet. Chromatographic separation was on an ODS Hypersil C(18) column using 0.05 M potassium dihydrogen phosphate buffer (pH 3.25, adjusted with orthophosphoric acid) and acetonitrile (82:18, v/v) as the mobile phase at a flow rate of 1.5 mL/min with detection at 210 nm. The asymmetry factors are 1.36 +/- 0.04 for fluconazole and 1.26 +/- 0.07 for tinidazole with a total run time of less than 7 min. The calibration curves were linear in the range 6-14 microg/mL for fluconazole and 80-190 microg/mL for tinidazole. The method was validated with respect to linearity, precision, accuracy, and specificity. The mean recovery for fluconazole and tinidazole is 99.65 +/- 0.84 and 99.34 +/- 0.70, respectively. The utility of the procedure is verified by its application to the market formulation that was subjected to various stressed conditions. Two potential degradation products of tinidazole on exposure to alkaline stressed condition are well-resolved. The method separated the two target drugs and degradation products well. No chromatographic interference is observed.
建立了一种快速灵敏的反相高效液相色谱法，用于同时测定复方片剂中口服活性三唑类抗真菌药氟康唑和属于5-硝基咪唑类的替硝唑。色谱分离在ODS Hypersil C(18)柱上进行，以0.05 M磷酸二氢钾缓冲液（用正磷酸调节pH至3.25）和乙腈（82:18，v/v）作为流动相，流速为1.5 mL/min，检测波长为210 nm。氟康唑的不对称因子为1.36±0.04，替硝唑的不对称因子为1.26±0.07，总运行时间少于7分钟。氟康唑的校准曲线在6 - 14 μg/mL范围内呈线性，替硝唑的校准曲线在80 - 190 μg/mL范围内呈线性。该方法在线性、精密度、准确度和专属性方面得到了验证。氟康唑和替硝唑的平均回收率分别为99.65±0.84和99.34±0.70。通过将该方法应用于经受各种强化条件的市售制剂，验证了该方法的实用性。替硝唑在碱性强化条件下暴露时的两种潜在降解产物得到了很好的分离。该方法能很好地分离两种目标药物和降解产物。未观察到色谱干扰。
