Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16412
標題: 電極萃取技術結合質譜術之應用
Application of Electrode Extraction coupled to Mass Spectrometry
作者: 楊宗杰
Yang, Tzung-Jie
關鍵字: electrode extraction
電極萃取
mass spectrometry
質譜術
出版社: 化學系所
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摘要: 本研究主要是發展電極萃取法,配合液相層析質譜儀的分析技術,檢測尿液中肌酸酐化合物與環境水樣中巴拉松化合物。 在肌酸酐檢測部分,實驗結果顯示電極萃取技術於磷酸鹽電解質溶液中具有較佳的萃取效果,控制電解質溶液pH為3,預氧化電位+1.6 V,預氧化時間150秒,磁石攪拌速率972 rpm,以線上模式(on-line mode),於脫附腔中注入100 μL超純水靜態脫附1分鐘,並結合液相層析儀之動相動態脫附1分鐘,進入液相層析管柱分離後,以電灑游離法正離子模式進行偵測。應用此技術於水中肌酸酐化合物之偵測,其線性範圍為0.5-10 μg/mL,線性相關係數為0.9984,偵測極限可達0.4 μg/mL,精密度為12.5 %,相對回收率為98.4 %。並應用此技術於真實尿液樣品之偵測,將尿液樣品以pH 3磷酸鹽電解質溶液稀釋250倍,測得尿液中肌酸酐含量為1.66 mg/mL。 在巴拉松檢測部分,實驗結果顯示電極萃取技術是以0.1N HCl將水溶液酸化,分別控制水溶液pH為2,預濃縮電位-0.6 V,預濃縮時間60秒,磁石攪拌速率858 rpm,以線上模式(on-line mode)結合液相層析儀之動相動態脫附3分鐘,進入液相層析管柱分離後,以大氣壓化學游離法正離子模式進行偵測。應用此技術於水中巴拉松化合物之偵測,其線性範圍為50-1000 ng/mL,線性相關係數為0.9991,偵測極限可達3 ng/mL,精密度在2.6-19 % 之間,相對回收率在74.2-101 % 之間。
In this study, we developed electrode extraction method coupled to liquid chromatography-mass spectrometry (LC-MS) to determine the amount of creatinine in human urine and parathion in environmental water sample. In creatinine study, extraction performed by electrode extraction at optimized conditions of preanodization potentional of +1.6V for 150s. The limit of detection for creatinine obtained in ultra pure water was 0.4 μg/mL. According to the analysis, the linear range was 0.5-10 μg/mL. To decrease the effect of matrix, in real sample analysis, the urine was diluted with pH 3 phosphate buffer solution to form ratio of 1:250 (v/v). The feasibility of applying the methods to determine creatinine in real samples was evaluated by analyzing urines sample from human. The relative recovery of creatinine was 98.4 %. The creatinine determined in urine samples was 1.66 mg/mL. Electrode extraction combined with liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI/MS/MS) was used to determine the trace levels of parathion in river water and ground water. In extraction preconcentration potentional was at -0.6V and preconcentration for 60s. Then the analytes were desorbed with dynamic desorption in modified SPME/HPLC desorption chamber for 3 min and determined with LC-APCI/MS/MS. From results show, the linear range is from 50 to 1000 ng/mL. The limit of detection for parathion in water was 3 ng/mL. The relative recovery of parathion was between 74.2 and 101 %.
URI: http://hdl.handle.net/11455/16412
其他識別: U0005-0206200611180700
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