Department of Medicinal Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, Egypt.
Department of Medicinal Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, Egypt; Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Horus University in Egypt, New Damietta, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2018 Nov 5;204:464-474. doi: 10.1016/j.saa.2018.06.078. Epub 2018 Jun 21.
A rapid, and highly sensitive analytical method were developed for the simultaneous determination of indacaterol maleate (IND) and glycopyrronium bromide (GLY) in their inhaler capsules. Valid ion-pairing chromatographic (IPC) method was performed for separation of GLY in presence of IND using C column and mobile phase consisting of acetonitrile: acidified deionized water (60:40% v/v) containing 0.02% sodium dodecyl sulfate (SDS) adjusted to pH 3.0 using OPA (orthophosphoric acid) isocratically eluted at 2.0 mL/min. Quantitation was achieved with UV detection at 210 nm. Cyproheptadine was used as an internal standard. The retention times were 1.9 and 2.5 min for IND, and GLY, respectively. For the IPC method, the calibration graphs were linear in the range of 0.66-66.0 μg/mL for IND and 0.3-30.0 μg/mL for GLY. The proposed method are rapid, reproducible (R.S.D. <2.0%) and achieves satisfactory resolution between IND and GLY (resolution factor = 4.23). The mean recoveries of the analytes in their inhaler capsule were satisfactory. It was applied successfully to in vitro dissolution testing using Franz diffusion cell and extended to a content uniformity test consistent with the United States Pharmacopoeia (USP) guidelines and were found to be precise and accurate for the capsules studied with acceptance value of 4.53 and 1.39 for IND and GLY, respectively.
建立了一种同时测定马来酸茚达特罗（IND）和格隆溴铵（GLY）吸入胶囊中这两种成分的快速、高灵敏度的分析方法。在存在 IND 的情况下，使用 C 柱和包含乙腈：酸化去离子水（60:40%v/v）的流动相（其中含有 0.02% 十二烷基硫酸钠（SDS），并用邻苯二甲醛（OPA）调节 pH 值至 3.0）进行有效离子对色谱（IPC）分离。以 2.0 mL/min 的等度洗脱，在 210 nm 处进行紫外检测来定量。赛庚啶被用作内标。IND 和 GLY 的保留时间分别为 1.9 和 2.5 min。对于 IPC 方法，IND 的校准曲线在 0.66-66.0 μg/mL 的范围内呈线性，GLY 的校准曲线在 0.3-30.0 μg/mL 的范围内呈线性。该方法快速、重现性好（R.S.D. <2.0%），并能在 IND 和 GLY 之间达到令人满意的分离度（分离因子 = 4.23）。在吸入胶囊中的分析物的平均回收率令人满意。该方法成功地应用于使用 Franz 扩散池进行的体外溶出试验，并扩展到与美国药典（USP）指南一致的含量均匀度测试，结果表明该方法对所研究的胶囊具有良好的精密度和准确度，IND 和 GLY 的接受值分别为 4.53 和 1.39。
