臺灣博碩士論文加值系統

中文摘要
本研究利用衍生反應配合氣相層析（gas chromatography，GC），對於抗高血壓藥物－enalapril，建立一簡單及具選擇性之定量分析法。
使用溴化五氟甲苯（pentafluorobenzyl bromide，PFBBr）為衍生試劑，將極性高、難揮發的enalapril之羧酸基衍生為酯，降低極性，在鹼催化下使成具適當揮發性之衍生物，再以GC分析。衍生反應設計為勻相反應，碳酸鉀為催化劑，將enalapril衍生後，利用固定相為SE-54毛細層析管來分離，以氫焰離子化型檢測器（flame ionization detector，FID）偵測，可定量70~875 nmol範圍之enalapril，最低檢測極限為17.5 nmol（S/N=3）。本研究對影響enalapril衍生反應之諸多因素：如反應之溶媒、衍生試劑需要量、反應溫度及反應時間、催化劑種類及需要量皆詳加探討。應用此方法於錠劑之分析可做為原料及製劑之品質管制。

英文摘要
A capillary gas chromatographic method is described for the determination of enalapril, an angiotension-converting enzyme inhibitor (ACEI). The method is based on the derivatization of enalapril with pentafluorobenzyl bromide (PFBBr) in acetone, using potassium carbonate as a base catalyst. Under the mild condition, the highly polar and nonvolatile enalapril was derivatized into a derivative with suitable chromatographic properties. The resulting derivative was separated on an SE-54 capillary column and determined by GC with a flame-ionization detector (FID).
Several parameters affecting the derivatization of enalapril including reaction solvent, the amount of derivatizating agent, the kind and amount of catalyst and reaction temperature and time were optimized. The method was simple and selective. The linear range of the method for the determination of enalarpil was 70~875 nmol. The detection limit (signal to noise ratio of 3) of enalapril in 350 mL acetone solution was at about 17.5 nmol.
Application of the method to the analysis of enalapril in tablets was proved to be feasible.

目 錄
英文摘要…………………………………………………………... i
中文摘要…………………………………………………………... ii
第一節 緒論…………………………………………………….. 1
第二節 實驗部分………………………………………………. 8
壹、 試藥及材料…………………………………………… 8
貳、 試藥溶液之配製……………………………………... 10
參、 儀器…………………………………………………….. 13
肆、 氣相層析條件………………………………………… 14
伍、 Enalapril基本分析法之探討…………….………… 15
(一) 適當衍生反應條件之探討…………….…….. 15
(二) Enalapril檢量線之製定法…………………. 19
(三) 精密度之探討………………………………….. 20
(四) 安定性之探討…………………………………. 20
陸、 衍生物合成及構造之確認探討…………………… 21
柒、 衍生反應產率探討…………………………………... 24
捌、 錠劑應用分析……………………………………….. 26
(一) 檢品前處理之探討…………………………… 26
(二) 市售錠劑之含量分析………………………… 28
(三) 錠劑中含量均一度之探討…………….…….. 29
(四) 錠劑中添加Enalapril回收率之探討………. 29
(五) 選擇性之試驗法………………………………. 31
第三節 結果與討論…………………………………………… 32
壹、 Enalapril基本分析法之建立………………………. 32
(一) 適當衍生反應條件之建立…………………... 32
(二) Enalapril衍生物之GC-FID層析圖……… 38
(三) Enalapril檢量線之建立…………………….. 40
(四) 精密度…………………………………………… 41
(五) 衍生物之安定性………………………………. 44
貳、 衍生物構造之確認…………………………………... 45
參、 衍生反應之產率……………………………………... 50
肆、 錠劑應用分析………………………………………… 52
(一) 檢品前處理方法之選定……………………… 52
(二) 市售錠劑之含量分析………………………… 57
(三) 錠劑中之含量均一度………………………… 58
(四) 錠劑中添加Enalapril之回收率……………. 60
(五) 選擇性…………………………………………… 62
第四節 結論…………………………………………………….. 65
參考文獻…………………………………………………………... 68
附圖目錄…………………………………………………………... 71
附表目錄…………………………………………………………... 72

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