Department of Pharmaco-Bromatology, Section Medicinal Products, Scientific Institute of Public Health (IPH), J. Wytmansstraat 14, 1050 Brussels, Belgium.
J Pharm Biomed Anal. 2011 Sep 10;56(2):200-9. doi: 10.1016/j.jpba.2011.05.013. Epub 2011 May 19.
A fully validated UHPLC method for the identification and quantification of pharmaceutical preparations, containing paracetamol and/or acetyl salicylic acid, combined with anti-histaminics (phenylephrine, pheniramine maleate, diphenhydramine, promethazine) and/or other additives as quinine sulphate, caffeine or codeine phosphate, was developed. The proposed method uses a Waters Acquity BEH C18 column (2 mm × 100 mm, 1.7 μm) with a gradient using an ammonium acetate buffer pH 4.0 as aqueous phase and methanol as organic modifier. The obtained method was fully validated based on its measurement uncertainty (accuracy profile) and robustness tests. Calibration lines for all components were linear within the studied ranges. The relative bias and the relative standard deviations for all components were respectively smaller than 1.5% and 2%, the β-expectation tolerance limits did not exceed the acceptance limits of 10% and the relative expanded uncertainties were smaller than 5% for all of the considered components. A UHPLC method was obtained for the identification and quantification of these kind of pharmaceutical preparations, which will significantly reduce analysis times and workload for the laboratories charged with the quality control of these preparations.
建立了一种完全验证的 UHPLC 方法,用于识别和定量含有扑热息痛和/或乙酰水杨酸、与抗组胺药(苯肾上腺素、马来酸苯海拉明、盐酸苯海拉明、异丙嗪)和/或其他添加剂(如硫酸奎宁、咖啡因或磷酸可待因)的药物制剂。所提出的方法使用 Waters Acquity BEH C18 柱(2mm×100mm,1.7μm),梯度采用 pH 4.0 的乙酸铵缓冲液作为水相,甲醇作为有机改性剂。该方法基于其测量不确定度(准确度概况)和稳健性测试进行了全面验证。所有成分的校准曲线在研究范围内均呈线性。所有成分的相对偏差和相对标准偏差均小于 1.5%和 2%,β-期望公差限不超过 10%的验收限,所有考虑成分的相对扩展不确定度均小于 5%。获得了一种用于识别和定量这些药物制剂的 UHPLC 方法,这将显著减少负责这些制剂质量控制的实验室的分析时间和工作量。