- 學位論文
(Ⅰ)以高效能液相層析儀並於移動相中加入TBA試劑來分析無機 陰離子的混合物 (Ⅱ)利用高效能液相層析法建立中草藥紫苑的化學指紋圖譜
(Ⅰ) Determination of inorganic anion mixtures by means of the HPLC method and tetra-n-butylammonium salt as ion- pair reagent (Ⅱ) Utilizing the HPLC method to investigate the chemical fingerprint of Chinese herbs Ziyuan
摘要
第一部份： 本研究主要是發展出一種新的離子層析方法，針對無機陰離子之混合物 (iodate、bromate、nitrite、bromide和nitrate) 同時進行分析。此方法以離子對層析法（Ion-pair chromatography, IPC）的分離原理，結合紫外光吸收偵測器（UV/Vis Detector）進行偵測。選用逆相octadecylsilica (ODS)管柱作為分離管柱，以acetonitrile-TBA- CH3COOH作為移動相，針對移動相pH值、最適波長選擇、離子對試劑濃度、移動相中有機溶劑濃度等是影響滯留時間和分離效果的重要因素進行探討，找出並建立最適分析方法為同時檢測無機陰離子混合物提供一套快速、有效的檢測方式。 第二部份： 本實驗以高效能液相層析儀（HPLC）結合Photodiode Array (PDA) UV/Vis 偵測器，來進行不同產地中草藥紫苑的分析。將紫苑樣品的萃取液，以梯度沖提方式進行分離，比對不同波長（210、230、254、280nm）所偵測到的圖譜，由分析結果，選擇254nm作為最適合用來製作化學指紋圖譜的波長，並標定出相對比例含量較高的吸收波峰作為主要特徵波峰，藉由主要特徵波峰面積的差異性來建立化學指紋圖譜，及比較不同產地對於紫苑成分的影響。最後，再將實驗數據制定成化學指紋圖譜及雷達圖譜，此化學指紋圖譜如同藥材指紋身分證，以作為藥材品種、產地之參考依據。
並列摘要
PartⅠ A novel ion chromatographic method has been developed for the simultaneous analysis of the inorganic anions (iodate, bromate, nitrite, bromide and nitrate) in their mixture. The method is based on the ion-pair chromatographic separation followed by the ultraviolet absorption detection. The separation was achieved on the reverse phase octadecylsilica (ODS) column and acetonitrile-TBA-CH3COOH mobile phase containing tetra-n-butylammonium salt (TBA) as an ion-pairing reagent. The pH of the mobile phase, the optimal wavelength, the concentration of the ion-pairing reagent and the concentration of the organic solvent in the mobile phase are the important factors which affect the retention time and efficiency of the separation. Therefore, the optimal analytic method which was found out and established can provide a fast and efficient method for the simultaneous analysis of the inorganic anions. PartⅡ Our aim in this study is that by utilizing the high performance liquid chromatography combined with the photodiode array (PDA) UV/Vis detector for analyzing the Chinese herb “Ziyuan” which were came from different producing areas. The extracts of the Chinese herb Ziyuan were separated by the gradient elution method and then the chromatograms obtained were compared with the different wavelength 210nm, 230nm, 254nm, 280nm. According to the results, the chromatograms of 254nm wavelength was selected and made the optimal chemical fingerprint chromatogram. Besides, there were several characteristic peaks chosen by the different peak area. The characteristic peaks were established the chemical fingerprint atlas and compared the composition of the Chinese herb Ziyuan which were came from different producing areas. Finally, the data obtained from the chromatograms were made the chemical fingerprint and radar atlas of Chinese herb. This radar atlas is like the identification card of the Chinese herb which could provide the information of their sources and producing areas.