很快,简单,敏感,高效和稳定的反相高效液相色谱法用于估计对羟基苯甲酸丙酯,开发了药物液体口服制剂中的对羟基苯甲酸甲酯和苯甲酸钠。AWatersAcquityUPLCBEHC18,50×2.1mm,使用1.7μmi.d.柱进行色谱分离,其中0.1%高氯酸流动相用作溶剂A,0.1%高氯酸和甲醇的混合物比例为20:80(v/v),分别,实验以0.4ml/min的流速进行,检测波长为240nm。柱的隔室温度设定为40°C,注射体积设定为2μ1。研究的主要目的是开发一种单一的UPLC测定方法,用于盐酸异丙嗪和盐酸右美沙芬的口服溶液中的异丙嗪(活性成分)和防腐剂,其中含有异丙嗪(活性成分)和对羟基苯甲酸甲酯,对羟基苯甲酸丙酯和苯甲酸钠(防腐剂)。开发了一种右美沙芬HBr的测定方法,并通过另一种HPLC方法进行了验证。对于盐酸异丙嗪,药物和防腐剂在19.3分钟的保留时间洗脱,对羟基苯甲酸甲酯9.3分钟,对羟基苯甲酸丙酯18.9分钟,苯甲酸钠8.9分钟。按照国际协调会议指南ICHQ2B和USP<1225>的规定,对开发的方法进行了验证。分析参数验证了特异性/选择性,线性度准确度,坚固性和鲁棒性。盐酸异丙嗪的线性范围,对羟基苯甲酸甲酯,对羟基苯甲酸丙酯和苯甲酸钠分别为10-100、10-80、1.0-8.0和10-80μg/ml,分别,活性成分和防腐剂的相关系数为1.00。异丙嗪的回收率百分比,对羟基苯甲酸丙酯,对羟基苯甲酸甲酯,苯甲酸钠为100.0-100.2、99.0-100.3、99.5-98.0和99.0-100.0%。验证的分析方法证明了该方法的特殊性,精确,线性,准确,敏感,坚固而稳定,表明液体口服制剂中活性成分和所有防腐剂的定量。
A quick, simple, sensitive, efficient and stability-indicating reverse-phase ultraperformance liquid chromatographic method for the estimation of propylparaben, methylparaben and sodium benzoate in a pharmaceutical liquid oral formulation was developed. A Waters Acquity UPLC BEH C18, 50 × 2.1 mm, 1.7 μm i.d. column was used to perform chromatographic separation with a 0.1% perchloric acid mobile phase used as solvent A and a mixture of 0.1 % perchloric acid and methanol in the ratio 20:80 (v/v), respectively, as solvent B. The experiments were carried out at a flow rate of 0.4 ml/min and the detection wavelength was 240 nm. The compartment temperature of the column was set at 40°C and the injection volume was set at 2 μl. The main aim of the research was to develop a single UPLC assay method for promethazine (active ingredient) and preservatives in the oral solution of promethazine HCl and dextromethorphan HBr that contains promethazine (active ingredient) and methylparaben, propylparaben and sodium benzoate (preservatives). An assay of dextromethorphan HBr was developed and validated by another HPLC method. The drug and preservatives were eluted at retention times of 19.3 min for promethazine HCl, 9.3 min for methylparaben, 18.9 min for propylparaben and 8.9 min for sodium benzoate. Validation of the developed method was carried out as stated by the International Conference on Harmonization guidelines ICH Q2B and under USP<1225>. The analytical parameters verified specificity/selectivity, linearity, accuracy, ruggedness and robustness. The linearity ranges of promethazine HCL, methylparaben, propylparaben and sodium benzoate were 10-100, 10-80, 1.0-8.0 and 10-80 μg/ml, respectively, with a correlation coefficient of active ingredients and preservatives of 1.00. Percentage recoveries of promethazine, propylparaben, methylparaben, and sodium benzoate were 100.0-100.2, 99.0-100.3, 99.5-98.0 and 99.0-100.0%. The validated analytical method proves that the method is specific, precise, linear, accurate, sensitive, rugged and stable, indicating the quantification of the active ingredient and all preservatives in liquid oral formulations.