- 期刊
開發箭型固相微萃取方法對有機氯禁用農藥之測定
Method Development for Prohibited Organochlorine Pesticides Detection by Solid-Phase Microextraction Arrow
摘要
食安是現代人所重視的議題，農藥的使用也越來越受到關切，因此精準及快速的分析是符合這股潮流的目標。在本研究中，推選出三種不得檢出的含氯農藥-阿特靈、地特靈、安特靈，在使用具有較大固相微萃取纖維吸附後，以氣相層析質譜儀（Gas Chromatography-Mass Spectrometry，GC-MS）進行分析，探討在前處理使用相當少量溶劑的情況下，即進行農藥檢測的可行性。首先利用四種纖維：1.二乙烯基苯／聚二甲基矽氧烷（Divinylbenzene／Polydimethylsiloxane，DVB／PDMS）、2.聚二甲基矽氧烷（Polydimethylsiloxane，PDMS）、3.聚丙烯酸酯（Polyacrylate，PA）、4.廣範圍碳纖維／聚二甲基矽氧烷（Carbon Wide Range，（WR）／PDMS）及搭配樣品萃取分析條件如1.搖瓶溫度2.搖瓶時間和3.脫附時間。發現在Carbon Wide Range（WR）／PDMS纖維所建立的分析條件下： 搖瓶溫度90℃、搖瓶時間15分鐘及脫附時間1分鐘，對此三種農藥的分析有最大的層析積分面積結果。此外本次所選用的農藥為衛生福利部食品藥物管理署規定不得檢出的項目，因此本研究更進一步確認其偵測極限。在以蘋果、紅蘿蔔、白米及黃豆做為基質時，經由上述Carbon Wide Range（WR）／PDMS纖維所建立的分析方法，可以發現三種農藥除了安特靈在黃豆中有大於濃度20 ppb的定量極限，其餘的農藥皆可在規範的濃度以下即被偵測出。市售較大纖維體積的固相微萃取纖維可在只透過使用相當少量的溶劑（丙酮：正己烷（1 : 1，v／v））進行樣品前處理，這對未來在開發禁用農藥檢測上提供了更快速且精準的檢驗方法。
並列摘要
Food safety is a key issue for people nowadays and the application of pesticides has been attracted more and more concern. Therefore, precise and fast pesticide analysis becomes the goal for this trend. Applying the higher volume of solid-phase microextraction (SPME) fiber accessories (SPME Arrows) for gas chromatography-mass spectrometry analysis to investigate the accessibility for sample preparation procedure with a limited amount of solvent for pesticide analysis, three non-detected chlorine containing pesticides, aldrin, dieldrin and endrin, were chosen in this study. Four SPME Arrow fibers were chosen: 1. Divinylbenzene/Poly-dimethylsiloxane (DVB/ PDMS), 2. Polydimethylsiloxane (PDMS), 3. Polyacrylate (PA), 4. Carbon Wide Range (WR)/PDMS with various sampling conditions, such as 1. sample incubation temperature, 2. sample incubation time and 3. fiber desorption time. Based on the chromatogram data analyses among three pesticides, Carbon Wide Range (WR)/ PDMS fiber showed the highest integrated areas under sample incubation temperature at 90℃ for 15 minutes and fiber desorption time for one minute. The three pesticides must be non-detected under Taiwan Food and Drug Administration regulations, therefore, their detection limits were further investigated. Using apple, carrot, rice, and soybean, respectively, as sample matrix, only endrin showed its quantitation limit of above 20 ppb in the soybean matrix. The other pesticides in the study could all be detected below the regulated concentrations. According to this study, the higher fiber volume in SPME Arrow is a tool with great potential in developing a fast and limited solvent (acetone: hexane (1 : 1, v/v)) analytical method for regulated prohibited pesticides.