Department of Chemistry, Faculty of Arts and Science, Eskisehir Osmangazi University, 26480, Eskisehir, Turkey.
Lefke European University, Faculty of Pharmacy, Department of Analytical Chemistry, Lefka, Cyprus.
J Food Drug Anal. 2018 Apr;26(2):842-848. doi: 10.1016/j.jfda.2017.08.002. Epub 2017 Sep 22.
Indacaterol is a new inhaled ultra-long acting β-agonist. It has been recently approved in the European Union for the treatment of chronic obstructive pulmonary disease. This paper reports, for the first time, a method for the determination and validation of Indacaterol (IND) using an internal standard in capsules. Capillary electrophoretic separation was performed on an uncoated fused-silica capillary (50 cm effective length, 75 μm i.d.) and background electrolyte composed of 20 mmol L of sodium tetraborate buffer, 15% (v/v) methanol (pH = 10.0) with the application of 20 kV of potential; 10 s at 5 × 10 N m (50 mbar) of injection time; and wavelength of 200 nm and 25 °C of temperature. The linearity was evaluated in the range of 4.90 × 10 mol L (2.50 μg mL) and 3.94 × 10 mol L (20.00 μg mL), with R = 0.9993 for inter-day. LOD and LOQ values were 2.18 × 10 mol L (0.011 μg mL) and 7.25 × 10 mol L (0.037 μg mL) for inter-day, respectively. The precision values were 0.50-1.06% for intra-day and 2.12% for inter-day as RSD%. The accuracy was tested by the standard addition method with the recovery values being between 98.79 and 99.09 as percentages with RSD% interval of 0.01-0.80. The developed method was validated according to ICH guidelines. Indacaterol was successfully determined in Arcapta capsule dosage form by the validated CE method with a relative error of 0.28%. The result was within the requirements of the USP 34-NF29. Therefore, the validated method may be used for the determination of Indacaterol in its capsules in quality control laboratories.
茚达特罗是一种新型吸入性超长效β激动剂。最近，它在欧盟被批准用于治疗慢性阻塞性肺疾病。本文首次报道了一种使用胶囊内标准品测定和验证茚达特罗（IND）的方法。毛细管电泳分离在未涂层熔融石英毛细管（有效长度 50cm，内径 75μm）上进行，背景电解质由 20mmol·L 的四硼酸钠缓冲液、15%（v/v）甲醇（pH=10.0）组成，施加 20kV 电势；10s 时进样时间为 5×10 N·m（50mbar）；波长为 200nm，温度为 25°C。在 4.90×10 mol·L（2.50μg·mL）和 3.94×10 mol·L（20.00μg·mL）范围内进行线性评估，日内 R=0.9993。LOD 和 LOQ 值分别为 2.18×10 mol·L（0.011μg·mL）和 7.25×10 mol·L（0.037μg·mL），日内精密度分别为 0.50-1.06%和 2.12%。准确度通过标准加入法进行测试，回收率在 98.79-99.09%之间，相对标准偏差（RSD%）为 0.01-0.80。该方法根据 ICH 指南进行了验证。采用验证后的 CE 法成功测定了 Arcapta 胶囊中的茚达特罗，相对误差为 0.28%。结果在 USP 34-NF 29 的要求范围内。因此，该验证后的方法可用于质量控制实验室中茚达特罗胶囊的测定。
