Faculty of Science and Technology, Al-Quds University, East Jerusalem.
Saudi Pharm J. 2010 Apr;18(2):103-6. doi: 10.1016/j.jsps.2010.02.006. Epub 2010 Feb 13.
A simple, precise, and accurate method is developed and validated for the analysis of pseudophedrine hydrochloride, dextromethorphan hydrobromide, chlorpheniramine maleate, and paracetamol in tablet formulations. The method has shown adequate separation of the four ingredients from each other. Separation was achieved on a silica column (5 μm, 125 × 4.6 mm inner diameter) using a mobile phase consisting of methanol/ammonium dihydrogen phosphate buffer (90:10, v/v) at a flow rate of 1.0 ml/min and UV detection at 220 nm. This new method is validated in accordance with USP requirements for new methods for assay determination, which include accuracy, precision, selectivity, linearity and range, robustness and ruggedness. The current method demonstrates good linearity over the range of 0.15-0.45 mg/ml of pseudophedrine hydrochloride with r (2) of 0.996, and in the range of 0.075-0.225 mg/ml of dextromethorphan hydrobromide with r (2) of 0.992, and in the range of 0.01-0.03 mg/ml of chlorpheniramine maleate with r (2) of 0.994, and in the range of 0.25-0.75 mg/ml of paracetamol with r (2) of 0.991. The average recovery of the method is 99.7%, 98.6%, 98.1%, and 99.2% for pseudophedrine hydrochloride, dextromethorphan hydrobromide, chlorpheniramine maleate, and paracetamol, respectively. The degree of reproducibility of the results obtained as a result of small deliberate variations in the method parameters and by changing analytical operator has proven that the method is robust and rugged.
建立并验证了一种用于分析片剂制剂中盐酸伪麻黄碱、氢溴酸右美沙芬、马来酸氯苯那敏和对乙酰氨基酚的简单、精确和准确的方法。该方法已显示出能够将这四种成分彼此充分分离。分离是在硅胶柱（5μm，125×4.6mm 内径）上进行的，使用甲醇/磷酸二氢铵缓冲液（90:10，v/v）作为流动相，流速为 1.0ml/min，在 220nm 处进行紫外检测。该新方法按照 USP 对新方法测定的要求进行验证，包括准确度、精密度、选择性、线性和范围、稳健性和耐用性。目前的方法在盐酸伪麻黄碱 0.15-0.45mg/ml 的范围内显示出良好的线性，r (2) 为 0.996，在氢溴酸右美沙芬 0.075-0.225mg/ml 的范围内，r (2) 为 0.992，在马来酸氯苯那敏 0.01-0.03mg/ml 的范围内，r (2) 为 0.994，在对乙酰氨基酚 0.25-0.75mg/ml 的范围内，r (2) 为 0.991。该方法的平均回收率分别为盐酸伪麻黄碱 99.7%、氢溴酸右美沙芬 98.6%、马来酸氯苯那敏 98.1%和对乙酰氨基酚 99.2%。由于方法参数的微小故意变化和分析操作人员的变化而获得的结果的重现性程度证明该方法是稳健和耐用的。
