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以動力學法和加速揮發方式快速偵測樣品中的特定成分 = Rapid Scr...
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國立高雄大學應用化學系碩士班
以動力學法和加速揮發方式快速偵測樣品中的特定成分 = Rapid Screening of Selected Compound from Mixture by Kinetic Method and Accelerated-Vaporization Ambient Ionization (AVAI)
紀錄類型:
書目-語言資料,印刷品 : 單行本
並列題名:
Rapid Screening of Selected Compound from Mixture by Kinetic Method and Accelerated-Vaporization Ambient Ionization (AVAI)
作者:
張淨雲,
其他團體作者:
國立高雄大學
出版地:
[高雄市]
出版者:
撰者;
出版年:
民99[2010]
面頁冊數:
128面圖,表 : 30公分;
標題:
ADMA
標題:
kinetic method
電子資源:
http://handle.ncl.edu.tw/11296/ndltd/13304064265577387092
摘要註:
本論文主要在發展不需經由管柱分離即可以快速偵測樣品中特定成分的方法,所採用的策略可分為動力學法(kinetic method)和加速揮發游離方式(Accelerated-Vaporization Ambient Ionization,AVAI)兩種。不需進行樣品前處理以及管柱分離,動力學法成功的辨識了混合液中ADMA與SDMA兩種同分異構物,若是兩種同分異構物相對含量介於0.05~20之間,動力學法也可以粗略估算其個別含量。研究當中我們也測得ADMA與SDMA的氣相酸度(gas-phase acidity,ΔGacid)各為1361.6 kJ/mol和1361.2 kJ/mol。將動力學法結合標準品添加法分析尿液中ADMA與SDMA的含量,所得結果與文獻報導一致。動力學法可進一步應用於三個同分異構物的辨識,我們除了可以辨識methylpyridines、monosaccharides和hexosamine monosaccharides三種類別化合物其中個別的三個同分異構物,也對後兩者其中同分異構物做了初步的定量分析。為了降低以動力學法分析樣品時鹽類和高分子對分析物訊號的壓抑,我們另行開發以加速揮發游離法(Accelerated-Vaporization Ambient Ionization,AVAI)分析混合液中的有機小分子。AVAI裝置可直接裝設於現有ESI/APCI游離源上使用,若以APCI模式操作則只需開啟corona discharge即可,不需使用流動相而大為減少溶劑的耗量。比較以傳統電噴灑游離方式和AVAI分析含4-methylpyridinec和高鹽類濃度以及PEG界面活性劑的混合液,可以發現AVAI方式所得質譜圖全無鹽類和PEG的干擾。藉由樣品液體積(0.01~1 ml)、pH值、極性等條件的控制,可以選擇性的偵測混合物中的特定分析物,以及縮短偵測時間至1分鐘即可完成。研究中我們發現以AVAI偵測特定分析物時,除了沸點以外,pKa也有很大的影響,推斷pH值和極性對分析物的溶劑能(solvation energy)影響了它的揮發性。 Kinetic Method was applied to analyze ADMA and SDMA in urine without utilizing pretreatment and separation. The method can direct distinguish ADMA and SDMA in mixture. Moreover, it can provide preliminary result of quantity of both compounds, if the relative amount of two isomers is between 0.05 and 20. We also obtained the gas-phase acidity (ΔGacid) of ADMA and SDMA, which were 1361.6 kJ/mol and 1361.2 kJ/mol, respectively. Combined kinetic method with standard addition, the amount of ADMA and SDMA in urine we estimated is in consistent with published results. The kinetic method not only can distinguish two isomers, it but also successfully applied to analyze methylpyridines, monosaccharides, and hexosamine mono- saccharides, which each contained three isomers.Accelerated-vaporization ambient ionization (AVAI) was developed to eliminate matrix effect while utilizing the kinetic method. AVAI required no modification on ESI/APCI hardward that currently used on mass spectrometer. When the AVAI was operated under APCI mode, it only required to turn on corona discharge emitter without usage of solvent. No matrix interference was presented in AVAI mass spectrum of solution mixed with 4-methylpyridinec, 1 M NaCl, and PEG. By varying sample size, pH, and solvent, we can selected detect compound from sample in minutes. We noticed that pKa and boiling point of compound had a strong effect on detection of selected compound and concluded that the solvation energy is one of key factor for selectivity of compound.
以動力學法和加速揮發方式快速偵測樣品中的特定成分 = Rapid Screening of Selected Compound from Mixture by Kinetic Method and Accelerated-Vaporization Ambient Ionization (AVAI)
張, 淨雲
以動力學法和加速揮發方式快速偵測樣品中的特定成分
= Rapid Screening of Selected Compound from Mixture by Kinetic Method and Accelerated-Vaporization Ambient Ionization (AVAI) / 張淨雲撰 - [高雄市] : 撰者, 民99[2010]. - 128面 ; 圖,表 ; 30公分.
參考書目:面.
ADMAkinetic method
以動力學法和加速揮發方式快速偵測樣品中的特定成分 = Rapid Screening of Selected Compound from Mixture by Kinetic Method and Accelerated-Vaporization Ambient Ionization (AVAI)
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本論文主要在發展不需經由管柱分離即可以快速偵測樣品中特定成分的方法,所採用的策略可分為動力學法(kinetic method)和加速揮發游離方式(Accelerated-Vaporization Ambient Ionization,AVAI)兩種。不需進行樣品前處理以及管柱分離,動力學法成功的辨識了混合液中ADMA與SDMA兩種同分異構物,若是兩種同分異構物相對含量介於0.05~20之間,動力學法也可以粗略估算其個別含量。研究當中我們也測得ADMA與SDMA的氣相酸度(gas-phase acidity,ΔGacid)各為1361.6 kJ/mol和1361.2 kJ/mol。將動力學法結合標準品添加法分析尿液中ADMA與SDMA的含量,所得結果與文獻報導一致。動力學法可進一步應用於三個同分異構物的辨識,我們除了可以辨識methylpyridines、monosaccharides和hexosamine monosaccharides三種類別化合物其中個別的三個同分異構物,也對後兩者其中同分異構物做了初步的定量分析。為了降低以動力學法分析樣品時鹽類和高分子對分析物訊號的壓抑,我們另行開發以加速揮發游離法(Accelerated-Vaporization Ambient Ionization,AVAI)分析混合液中的有機小分子。AVAI裝置可直接裝設於現有ESI/APCI游離源上使用,若以APCI模式操作則只需開啟corona discharge即可,不需使用流動相而大為減少溶劑的耗量。比較以傳統電噴灑游離方式和AVAI分析含4-methylpyridinec和高鹽類濃度以及PEG界面活性劑的混合液,可以發現AVAI方式所得質譜圖全無鹽類和PEG的干擾。藉由樣品液體積(0.01~1 ml)、pH值、極性等條件的控制,可以選擇性的偵測混合物中的特定分析物,以及縮短偵測時間至1分鐘即可完成。研究中我們發現以AVAI偵測特定分析物時,除了沸點以外,pKa也有很大的影響,推斷pH值和極性對分析物的溶劑能(solvation energy)影響了它的揮發性。 Kinetic Method was applied to analyze ADMA and SDMA in urine without utilizing pretreatment and separation. The method can direct distinguish ADMA and SDMA in mixture. Moreover, it can provide preliminary result of quantity of both compounds, if the relative amount of two isomers is between 0.05 and 20. We also obtained the gas-phase acidity (ΔGacid) of ADMA and SDMA, which were 1361.6 kJ/mol and 1361.2 kJ/mol, respectively. Combined kinetic method with standard addition, the amount of ADMA and SDMA in urine we estimated is in consistent with published results. The kinetic method not only can distinguish two isomers, it but also successfully applied to analyze methylpyridines, monosaccharides, and hexosamine mono- saccharides, which each contained three isomers.Accelerated-vaporization ambient ionization (AVAI) was developed to eliminate matrix effect while utilizing the kinetic method. AVAI required no modification on ESI/APCI hardward that currently used on mass spectrometer. When the AVAI was operated under APCI mode, it only required to turn on corona discharge emitter without usage of solvent. No matrix interference was presented in AVAI mass spectrum of solution mixed with 4-methylpyridinec, 1 M NaCl, and PEG. By varying sample size, pH, and solvent, we can selected detect compound from sample in minutes. We noticed that pKa and boiling point of compound had a strong effect on detection of selected compound and concluded that the solvation energy is one of key factor for selectivity of compound.
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http://handle.ncl.edu.tw/11296/ndltd/13304064265577387092
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