Usman Shahnaz, Akram Muhammad, Aziz Asif, Ramesh Venkat, Sarheed Omar Abdulraheem
RAK College of Pharmaceutical Sciences, RAK Medical and Health Sciences University, Ras Al Khaimah, UAE / Department of Pharmaceutics, Faculty of Pharmacy, University of Karachi, Karachi, Pakistan.
Department of Pharmaceutics, Faculty of Pharmacy, University of Karachi, Karachi, Pakistan.
Pak J Pharm Sci. 2014 Sep;27(5 Spec no):1541-6.
The aim of the present study was to develop and validate an analytical method for the estimation of nepafenac as a raw material as well as in dosage form (suspension) by using reverse phase high performance liquid chromatographic (RP-HPLC). The target was to obtain an easy, rapid, reproducible as well as a rugged method. The HPLC system that was used in the proposed study was LC-20AD liquid chromatograph equipped with SPD-20A UV-VIS detector. The separation was performed on C18 column which was attached with loop 20 β l. Elution was done at ambient temperature with a mobile phase consisting of acetonitrile: Water (40: 60v/v) at a flow rate of 1ml/min and at a wavelength of 254 nm. The proposed method was validated as per the ICH guidelines. The retention time for nepafenac was 7.49 minutes (% CV=0.0076). The percentage coefficient variation (CV) of six consecutive peak areas of injections was 0.34% with tailing factor 1.76. The peak area responses were linear within the concentration range of 0.078-20.0 βg/ml (R(2)=0.9993). The sensitivity of the method could be evaluated by limits of detection (LOD) (0.0195 β g/ml) and limits of quantitation (LOQ) (0.039 β g/ml). Nepafenac drug is s in its diluent that could see by intra-day (% CV =0.45-1.96) and inter-day variation (%CV=0.173-1.898%). The accuracy and recovery results of 80%, 100% and 120% were 97.40% to 102.10% with % CV of 0.3201% to 1.3496%. The robustness and ruggedness of the method are significantly broader and is reproducible. It could be used as a more convenient, efficient, easy and time saving method for the analysis of drug in raw material as well as in dosage form (ophthalmic suspension).
本研究的目的是开发并验证一种采用反相高效液相色谱法（RP-HPLC）测定萘非那啶原料药及其剂型（混悬剂）的分析方法。目标是获得一种简便、快速、可重现且耐用的方法。本研究所使用的HPLC系统为配备SPD-20A紫外-可见检测器的LC-20AD液相色谱仪。分离在连接20 μl定量环的C18柱上进行。在室温下，以乙腈:水（40:60 v/v）为流动相，流速为1 ml/min，在254 nm波长下进行洗脱。所提出的方法按照国际协调会议（ICH）指南进行了验证。萘非那啶的保留时间为7.49分钟（% CV = 0.0076）。进样六次连续峰面积的百分比变异系数（CV）为0.34%，拖尾因子为1.76。峰面积响应在0.078 - 20.0 μg/ml的浓度范围内呈线性（R² = 0.9993）。该方法的灵敏度可通过检测限（LOD）（0.0195 μg/ml）和定量限（LOQ）（0.039 μg/ml）来评估。萘非那啶药物在其稀释剂中的日内变异（% CV = 0.45 - 1.96）和日间变异（% CV = 0.173 - 1.898%）均可接受。80%、loo%和120%加样回收率的准确度结果为97.40%至102.10%，% CV为0.3201%至1.3496%。该方法的耐用性和重现性显著更高且可重现。它可作为一种更方便、高效、简便且省时的方法，用于分析原料药及剂型（眼用混悬剂）中的药物。
