DemİrtÜrk Esra, Nemutlu Emirhan, Şahİn Selma, Öner Levent
Department of Pharmaceutical Technology, Faculty of Pharmacy, Çukurova University Turkey.
Department of Pharmaceutical Technology, Faculty of Pharmacy, Hacettepe University Turkey.
Turk J Chem. 2020 Jun 1;44(3):647-655. doi: 10.3906/kim-1912-45. eCollection 2020.
A simple and reliable HPLC method was developed and validated for determination of rofecoxib in bovine serum albumin microsphere. The analyses were performed on a C18 column (150 x 4.6 mm, 5 μm particle size) at room temperature with UV detection at 272 nm. The mobile phase was composed of acetonitrile-0.1% o-phosphoric acid solution in water (1:1, v/v) mixture, and flow rate was set to 1 mL/min. The method was validated according to the international guidelines with respect to stability, linearity range, limit of quantitation and detection, precision, accuracy, specificity, and robustness. The detection and quantification limit of the method were 1.0 μg/mL and 2.5 μg/mL, respectively. The method was linear in the range of 2.5-25 μg/mL with excellent determination coefficients (R2 >0.99). Intra-day and inter-day precision (<1.76% RSD) and accuracy (<0.55 % Bias) values of the method also fulfilled the required limits. It was concluded that the developed method was accurate, sensitive, precise, and reproducible according to the evaluation of the validation parameters. The applicability of the method was confirmed for in vitro quantification of rofecoxib in bovine serum albumin microspheres.
建立并验证了一种简单可靠的高效液相色谱法,用于测定牛血清白蛋白微球中的罗非昔布。分析在室温下于C18柱(150×4.6 mm,粒径5μm)上进行,采用272 nm紫外检测。流动相由乙腈-0.1%磷酸水溶液(1:1,v/v)混合物组成,流速设定为1 mL/min。该方法根据国际指南在稳定性、线性范围、定量限和检测限、精密度、准确度、特异性和稳健性方面进行了验证。该方法的检测限和定量限分别为1.0μg/mL和2.5μg/mL。该方法在2.5-25μg/mL范围内呈线性,测定系数良好(R2>0.99)。该方法的日内和日间精密度(RSD<1.76%)和准确度(偏差<0.55%)值也符合要求的限度。根据验证参数的评估得出结论,所建立的方法准确、灵敏、精密且可重现。该方法在体外定量牛血清白蛋白微球中罗非昔布的适用性得到了证实。