臺灣博碩士論文加值系統

本研究為利用衍生反應配合毛細管－氣相層析，對抗組織胺藥物 cetirizine建立一簡單、敏感及準確之微量分析法。本方法為在氰甲烷溶液中，利用溴化五氟甲苯 (PFBBr) 為衍生試劑，以碳酸鉀為鹼催化劑，在溫和條件下，將高極性、不具揮發性之 cetirizine衍生為具適當層析性質之衍生物。所得之衍生物以 SE-54 毛細層析管分離，再以火焰離子檢測器 (FID) 偵測。
影響衍生反應之一些因素，如：反應溶媒、衍生試劑需要量、鹼催化劑之選擇及用量及反應溫度、時間等，皆詳加討論。本建立之分析法，檢量線定量範圍為： cetirizine 10-200 nmol ；檢出極限 (訊號對雜訊比為 5) 為在0.2 mL氰甲烷溶液中大約 2 nmol之cetirizine。此分析法將可應用於製劑檢品之分析。

A capillary gas chromatographic method is described for the determination of trace cetirizine. The method is based on the derivatization of cetirizine with pentafluorobenzyl bromide in acetonitrile using potassium carbonate as a base catalyst. Under a mild condition, the highly polar and nonvolatile cetirizine was derivatized into derivative with suitable gas chromatographic properties. The derivative of cetirizine was separated on a SE-54 capillary column and detected by a flame-ionization detector.
Several parameters affecting the derivatization of cetirizine were investigated. The linear range of the method for the determination of cetirizine was over 10-200 nmol. The detection limit (signal to noise ratio of 5) of cetirizine in 0.2 mL acetonitride solution was about 2 nmol. Application of the method to the analysis of cetirizine in tablets will be feasible.

附圖目錄 -------------------------------------------------- Ⅲ
附表目錄 -------------------------------------------------- Ⅳ
英文摘要 -------------------------------------------------- 1
中文摘要 -------------------------------------------------- 2
第一節 緒論 --------------------------------------------- 3
第二節 實驗部分 ----------------------------------------- 7
壹、 試藥及材料 --------------------------------------- 7
貳、 試藥溶液之配製 ----------------------------------- 8
參、 儀器 --------------------------------------------- 11
肆、 氣相層析條件 ------------------------------------- 12
伍、 Cetirizine基本分析法之探討 ----------------------- 13
(一) 適當衍生反應條件之探討 ---------------------- 13
(二) Cetirizine檢量線之製定法 -------------------- 17
(三) 精密度之探討 -------------------------------- 18
(四) 安定性之探討 -------------------------------- 19
陸、 衍生物合成及構造之確認探討 ----------------------- 20
柒、 錠劑應用分析 ------------------------------------- 22
(一) 檢品前處理之探討 ---------------------------- 22
(二) 市售錠劑之含量分析 -------------------------- 24
(三) 錠劑中含量均一度之探討 ---------------------- 25
(四) 錠劑中添加cetirizine回收率之探討 ------------ 25
第三節 結果與討論 --------------------------------------- 27
壹、 Cetirizine基本分析法之建立 ----------------------- 27
(一) 適當衍生反應條件之建立 ---------------------- 27
(二) Cetirizine衍生物之GC-FID層析圖 ------------- 33
(三) Cetirizine檢量線之建立 --------------------- 35
(四) 精密度 -------------------------------------- 36
(五) 衍生物之安定性 ------------------------------ 39
貳、 衍生物構造之確認 --------------------------------- 40
參、 錠劑應用分析 ------------------------------------- 42
(一) 檢品前處理方法之選定 ------------------------ 42
(二) 市售錠劑之含量分析 -------------------------- 46
(三) 錠劑中之含量均一度 -------------------------- 46
(四) 錠劑中添加cetirizine之回收率 ---------------- 49
肆、 電子捕獲型氣相層析對cetirizine之微量分析初步探討-- 51
第四節 結論 --------------------------------------------- 54
參考文獻 -------------------------------------------------- 56

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