Jahan Md Sarowar, Islam Md Jahirul, Begum Rehana, Kayesh Ruhul, Rahman Asma
Department of Biochemistry and Molecular Biology, University of Dhaka, Dhaka, Bangladesh.
Department of Chemistry, University of Dhaka, Dhaka, Bangladesh.
Anal Chem Insights. 2014 Nov 18;9:75-81. doi: 10.4137/ACI.S18651. eCollection 2014.
A rapid and stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous quantification of paracetamol and ibuprofen in their combined dosage form especially to get some more advantages over other methods already developed for this combination. The method was validated according to United States Pharmacopeia (USP) guideline with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity, and system suitability. Forced degradation study was validated according to International Conference on Harmonisation (ICH). For this, an isocratic condition of mobile phase comprising phosphate buffer (pH 6.8) and acetonitrile in a ratio of 65:35, v/v at a flow rate of 0.7 mL/minute over RP C18 (octadecylsilane (ODS), 150 × 4.6 mm, 5 μm, Phenomenex Inc.) column at ambient temperature was maintained. The method showed excellent linear response with correlation coefficient (R (2)) values of 0.999 and 1.0 for paracetamol and ibuprofen respectively, which were within the limit of correlation coefficient (R (2) > 0.995). The percent recoveries for two drugs were found within the acceptance limit of (97.0-103.0%). Intra-and inter-day precision studies of the new method were less than the maximum allowable limit percentage of relative standard deviation (%RSD) ≤ 2.0. Forced degradation of the drug product was carried out as per the ICH guidelines with a view to establishing the stability-indicating property of this method and providing useful information about the degradation pathways, degradation products, and how the quality of a drug substance and drug product changes with time under the influence of various stressing conditions. The degradation of ibuprofen was within the limit (5-20%, according to the guideline of ICH), while paracetamol showed <20% degradation in oxidation and basic condition.
建立了一种快速且具有稳定性指示作用的反相高效液相色谱（RP-HPLC）方法，用于同时定量扑热息痛和布洛芬的复方制剂，特别是相对于已开发的其他该复方制剂方法具有更多优势。该方法根据美国药典（USP）指南在准确性、精密度、特异性、线性、溶液稳定性、稳健性、灵敏度和系统适用性方面进行了验证。强制降解研究根据国际协调会议（ICH）进行了验证。为此，在室温下，于RP C18（十八烷基硅烷（ODS），150×4.6 mm，5μm，菲罗门公司）柱上，以0.7 mL/分钟的流速保持流动相的等度条件，流动相由磷酸盐缓冲液（pH 6.8）和乙腈按65:35（v/v）的比例组成。该方法显示出优异的线性响应，扑热息痛和布洛芬的相关系数（R(2)）值分别为0.999和1.0，均在相关系数限度（R(2)>0.995）内。两种药物的回收率百分比在（97.0 - 103.0%）的可接受限度内。新方法的日内和日间精密度研究小于相对标准偏差（%RSD）≤2.0的最大允许限度百分比。按照ICH指南对药品进行强制降解，以确立该方法的稳定性指示特性，并提供有关降解途径、降解产物以及在各种应激条件影响下原料药和药品质量如何随时间变化的有用信息。布洛芬的降解在限度内（根据ICH指南为5 - 20%），而扑热息痛在氧化和碱性条件下显示<20%的降解。
