Güray Tufan, Turan Tugba, Tunçel Muzaffer, Uysal Ulku Dilek
Eskisehir Osmangazi University, Faculty of Arts and Science, Department of Chemistry, Eskisehir, Turkey.
Lefke European University, Faculty of Pharmacy, Department of Analytical Chemistry, Lefka, Turkish Republic of Northern Cyprus.
J AOAC Int. 2017 Jan 1;100(1):206-211. doi: 10.5740/jaoacint.16-0201.
A validated rapid and sensitive capillary zone electrophoretic method for the determination of olopatadine hydrochloride (OLO) is described. Optimum conditions were found: 20 mmol/L sodium tetraborate buffer, acetonitrile 15% (v/v), 10 mmol/L NaCl at pH 9.5, with 25 kV of applied potential, injection time of 10 s at 5 × 103 N/m2, at a wavelength of 205 nm, and fixed temperature of 30°C. The calibration curve was linear in the range of 1.13 × 10-5 mol/L (4.22 μg/mL) to 5.65 × 10-5 mol/L (21.12 μg/mL), with R = 0.9995 for interday precision. LOD and LOQ values were 1.58 × 10-6 (0.58 μg/mL) and 4.78 × 10-6 mol/L (1.75 μg/mL), respectively. Precision values were 1.10-1.97% for intraday and 1.41% for interday RSDs. Accuracy was tested by preparing a synthetic mixture whose composition was similar to the pharmaceutical preparation for Patanol. The RSDs of the recovery values (98.2%) were between 0.42 and 0.65% and the amount of OLO found was 1.09 mg/mL. The result was within the requirements of USP 31-NF 26. Therefore, this validated method is suggested for routine analysis for the determination of OLO in laboratories.
本文描述了一种经验证的快速灵敏的毛细管区带电泳法，用于测定盐酸奥洛他定（OLO）。研究发现了最佳条件：20 mmol/L硼酸钠缓冲液、15%（v/v）乙腈、10 mmol/L氯化钠，pH值为9.5，施加电压25 kV，在5×103 N/m2压力下进样10 s，检测波长205 nm，固定温度30°C。校准曲线在1.13×10-5 mol/L（4.22 μg/mL）至5.65×10-5 mol/L（21.12 μg/mL）范围内呈线性，日间精密度R = 0.9995。检测限（LOD）和定量限（LOQ）分别为1.58×10-6（0.58 μg/mL）和4.78×10-6 mol/L（1.75 μg/mL）。日内精密度RSD值为1.10 - 1.97%，日间为1.41%。通过制备一种组成与帕坦洛药物制剂相似的合成混合物来测试准确度。回收率（98.2%）的RSD在0.42%至0.65%之间，测得的OLO量为1.09 mg/mL。结果符合美国药典31 - 国家处方集26的要求。因此，建议采用这种经验证的方法在实验室进行OLO的常规分析。
