Hassib Sonia Talaat, Mohammad Mohammad Abdul-Azim, El-Zaher Asmaa A, El-Kady Ehab F
Cairo University, Faculty of Pharmacy, Department of Pharmaceutical Chemistry, Kasr El-Aini 11562, Cairo, Egypt.
J AOAC Int. 2007 May-Jun;90(3):693-9.
New, simple, rapid, and precise reversed-phase high-performance liquid chromatographic (LC) methods were developed for the simultaneous determination of chlorzoxazone (CH) and ketoprofen (KT) in binary mixtures and in ternary mixtures containing the CH degradation product, 2-amino-4-chlorophenol (CD). The analytes were separated by LC on a Lichrosphere 60 C18 column (250 x 4 mm, 5 microm). The mobile phases, methanol-water (40:60, v/v) at 1 mL/min and methanol-0.05% phosphoric acid (60:40, v/v, pH 2.81) at 1.5 mL/min, satisfactorily resolved the binary and ternary mixtures, respectively. The UV detector was operated at 280 nm for the determination of CH and at 254 nm for the determination of KT and CD. Linearity, accuracy, and precision were found to be acceptable over the concentration ranges of 20-240 and 5-60 microg/mL for CH and KT, respectively, in the binary mixtures and 50-300, 10-60, and 20-160 microg/mL for CH, KT, and CD, respectively, in the ternary mixtures. The optimized methods proved to be specific, robust, and accurate for the quality control of CH and KT in pharmaceutical preparations.
开发了新的、简单、快速且精确的反相高效液相色谱（LC）方法，用于同时测定二元混合物以及含有氯唑沙宗（CH）降解产物2-氨基-4-氯苯酚（CD）的三元混合物中的氯唑沙宗（CH）和酮洛芬（KT）。分析物在Lichrosphere 60 C18柱（250×4 mm，5微米）上通过液相色谱分离。流动相，甲醇-水（40:60，v/v），流速1 mL/min，以及甲醇-0.05%磷酸（60:40，v/v，pH 2.81），流速1.5 mL/min，分别能令人满意地分离二元和三元混合物。紫外检测器在280 nm处用于测定CH，在254 nm处用于测定KT和CD。在二元混合物中，CH和KT的浓度范围分别为20 - 240和5 - 60 μg/mL，在三元混合物中，CH、KT和CD的浓度范围分别为50 - 300、10 - 60和20 - 160 μg/mL时，线性、准确度和精密度均被认为是可接受的。优化后的方法被证明对药物制剂中CH和KT的质量控制具有特异性、稳健性和准确性。
