Saokham Phennapha, Loftsson Thorsteinn
Faculty of Pharmaceutical Sciences, University of Iceland Reykjavík Iceland.
Faculty of Pharmaceutical Sciences, University of Iceland Reykjavík Iceland.
J Pharm Sci. 2015 Nov;104(11):3925-3933. doi: 10.1002/jps.24608. Epub 2015 Aug 6.
Fast and simple high-pressure liquid chromatographic (HPLC) method with charged aerosol detector (CAD) was developed for quantitation of γ-cyclodextrin (γCD) in aqueous solutions. The chromatographic system consisted of a C18 column (i.e., the stationary phase) and an aqueous mobile phase containing 7% (v/v) methanol. Calibration curve was obtained over the γCD concentration range of 0.005%-1% (w/v). The limit of detection and quantitation of γCD were 0.0001% and 0.0002% (w/v), respectively. Formation of γCD aggregates in aqueous solution and their critical aggregation concentration (cac) were determined by both conventional dynamic light scattering method and permeation method using HPLC-CAD for quantitative determination of γCD. The cac of γCD was determined to be 0.95% (w/v) and the amount of γCD self-aggregates increased with increasing γCD concentrations. Also, the developed HPLC-CAD method was used to determine the γCD phase-solubility profile in an aqueous hydrocortisone (HC)/γCD complexation medium. The maximum concentration of dissolved γCD and HC was determined to be 1.47% and 0.31% (w/v), respectively. The membrane permeation method was shown to be a reliable method for determination of metastable γCD aggregates. The HPLC-CAD method was successfully applied for quantitative determination of γCD in aqueous solutions during permeation and phase-solubility studies.
开发了一种采用带电气溶胶检测器（CAD）的快速简便的高压液相色谱（HPLC）方法，用于定量分析水溶液中的γ-环糊精（γCD）。色谱系统由一根C18柱（即固定相）和一种含有7%（v/v）甲醇的水性流动相组成。在γCD浓度范围为0.005%-1%（w/v）内获得校准曲线。γCD的检测限和定量限分别为0.0001%和0.0002%（w/v）。通过传统的动态光散射法和使用HPLC-CAD进行定量测定γCD的渗透法，测定了水溶液中γCD聚集体的形成及其临界聚集浓度（cac）。γCD的cac测定为0.95%（w/v），且γCD自聚集体的量随γCD浓度增加而增加。此外，所开发的HPLC-CAD方法用于测定氢化可的松（HC）/γCD水性络合介质中γCD的相溶解度曲线。溶解的γCD和HC的最大浓度分别测定为1.47%和0.31%（w/v）。膜渗透法被证明是测定亚稳态γCD聚集体的可靠方法。HPLC-CAD方法成功应用于渗透和相溶解度研究过程中水溶液中γCD的定量测定。
