纖維電噴灑游離質譜法結合線上微萃取濃縮技術對嘉磷塞的分析與研究

Applications of an on-line microextraction method for use in the analysis of glyphosate based on fiber-spray/mass spectrometry

王星翰(Wang Sing-Han)

指導教授 ： 林震煌

國立臺灣師範大學/理學院/化學系/碩士(2018年)

https://doi.org/10.6345/THE.NTNU.DC.005.2018.B05

摘要

為了分析嘉磷塞，本研究開發了結合線上微萃取濃縮技術及纖維電噴灑游離質譜法的方法，本研究利用2毫升樣品瓶（儲存樣品溶液）及一小段中空纖維管（用來進行萃取, 3.5公分長, 外徑/內徑, 1.0 mm/0.6 mm）製作裝置，此微萃取裝置可架設於電噴灑游離源與質譜口之間，分析物能利用中空纖維液相微萃取操作過程，從稀的溶液被提取出來，被提取出來的分析物會透過擴散移動到纖維外，濃縮的分析物被蒸發並通過多孔表面逸出，同時間，由電噴灑游離源產生帶電液珠，一旦來自中空纖維表面（大部分為中性）的蒸發物質遇到電噴霧，游離化便會發生。本實驗用於液相微萃取的液膜為體積比octanol：Aliquat 336：dodecane = 0.4：1：8.6，萃取溶液為0.1 M HCL，利用此方法最低偵測極限可以達到1 ng/mL。當使用攪拌子攪拌時，萃取時間可以從60分鐘減少至僅15分鐘。

關鍵字

嘉磷塞 ； 中空纖維 ； 液-液微萃取

並列摘要

For the analysis of glyphosate, a novel method based on the combination of on-line microextraction and fiber-spray/mass spectrometry was developed. A microextraction kit was designed for this purpose, in which a 2 mL sample vial (reservoir for the sample solution) and a piece of a porous polypropylene hollow fiber (for sample extraction; 3.5 cm in length; O.D./I.D., 1.0/0.6 mm, respectively) were used, respectively. The microextraction kit was located between the mass inlet and the ESI needle. Analytes can be extracted from a very dilute solution operating the so-called hollow fiber liquid phase microextraction process, and the resulting extract then moves to the outside portion of the fiber by diffusion. Following this, the concentrated analytes were evaporated and escape through the porous surface. Meanwhile, the electrosprayed/charged droplets are produced from a regular ESI stainless needle. Once the evaporated materials from the surface of the hollow fiber (mostly neutral) meet the electrospray plume, ionization occurs under ambient conditions. In order to process liquid-phase microextraction, the membrane solution (0.2 M Aliquat 336 in dodecane modified with 4% octanol) and an acceptor solution (0.1 M HCl) were used, respectively. Using the setup, it was possible to improve the limit of detection after microextraction by ∼1000-fold. The limit of detection achieved was 1 ng/mL. When a stir bar was used, the extraction time can be shortened from 60 min to only 15 min.

並列關鍵字

glyphosate ； hollow fiber ； liquid-liquid microextration

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