大體積樣品進樣及電極反轉技術之毛細管電泳分析法對類固醇吸入劑budesonide之分析研究

Determination of Budesonide by Large Volume Sample Stacking with Reverse Polarity in Capillary Electrophoresis

洪葦蓉(Wei-Jung Hung)

指導教授 ： 陳素惠

高雄醫學大學/藥學院/藥學研究所/碩士(2012年)

摘要

本論文之研究主題為利用大體積檢品進樣堆積以及電極反轉技術（Large Volume Sample Stacking with Reverse Polarity；LVSSRP）之毛細管電泳法來提高對類固醇吸入劑budesonide之偵測感度，並以donepezil作為內部標準品，建立一個簡單且同時具有選擇性之定量分析法。
本方法主要藉由注入大體積量之低濃度檢品溶液，在於毛細管內進行濃縮以及分析。首先，毛細管內先填充滿分析作業用緩衝溶液：50 mM 硼酸鹽（pH 9.0）、40 mM sodium dodecyl sulfate（SDS）、10% 甲醇，再以壓力方式注入大量檢品（5 psi，60秒），之後將電極反轉，並供予-5 kV的電壓，此時電滲透流會將檢品溶媒推擠出毛細管，待測物則堆積於緩衝溶液及檢品溶液之界面，即會在線上達濃縮效果，當電流回升至緩衝溶液應有電流之95%時，再將電極恢復成正常模式，並予以20 kV的電壓進行樣品分析。
本研究加以探討了影響分離的因素，包括：硼酸鹽緩衝溶液的pH值和濃度、SDS的濃度以及緩衝溶液中甲醇的含量，最後會將此分析方法應用於市售budesonide吸入劑之含量分析。

關鍵字

類固醇吸入劑 ； 大體積檢品進樣堆積 ； 電極反轉技術

並列摘要

This study describes approaches for stacking and analyzing glucocorticoid inhalation budesonide by large volume sample stacking (LVSS) with reverse polarity (RP) in capillary electrophoresis (CE).
After filling background solution (BGS) containing 50 mM borate buffer pH 9.0 with 40 mM sodium dodecyl sulfate (SDS) and 10% MeOH, large sample volume was loaded by hydrodynamic injection (5 psi, 60sec), followed by the removal of sample matrix from capillary using RP (-5 kV). Monitoring the current and normalizing the polarity when 95% of current recovered, the separation of neutral analytes was performed in the background solution under 20 kV and on-column detection at 230 nm. Removing most of electrolytes from sample solution is a key step for performing LVSS.
The linear range of the method for determination of the test drug, using donepezil as an internal standard (IS), was all over the range 0.3-5 μg/mL for budesonide. The application of the proposed method for determination the concentration of budesonide in drug formulations was demonstrated.

並列關鍵字

budesonide ； LVSS ； reverse polarity

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