以分散式液液微萃取技術結合基質輔助雷射脫附游離飛行時間質譜儀分析毛地黃毒苷化合物

Using Dispersive Liquid-Liquid Microextraction for the Determination of Digitoxin by Matrix Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

楊汶陵(Wenn-Ling Yang) ； 劉建忠(Chien-Chung Liou)

《東海科學》 12期 (2010/07) Pp. 29-44

https://doi.org/10.29723/TS.201007.0003

摘要

本論文以分散式液液微萃取法，針對樣品溶液中毛地黃毒苷的藥物成份，進行萃取與預濃縮的前處理步驟，再配合基質輔助雷射脫附游離飛行時間質譜儀，進行分析物的偵測。
將1mL的四氫呋喃分散劑與12μL的氯仿萃取劑，分別注入5mL的毛地黃毒苷標準溶液中，即呈現白色混濁狀，此時分析物通過分散劑被濃縮至萃取劑中，經過離心後，將離心管底部的沉澱液取出，並與α-CHCA基質溶液混合，再送入質譜儀做鑑定與分析。
由實驗結果得知，本論文所提出的分析方法，對於毛地黃毒苷的質譜訊號增強效果，最高約可達1,200倍以上，分析物在水溶液中的偵測極限爲2.2nM、線性範圍爲0.05~1μM、相關係數(R^2)值爲0.9998、相對標準偏差值均在10%以內。
此分析方法可成功地應用於尿液中毛地黃毒苷的檢驗，樣品溶液只需經過簡單的前處理步驟，即可進行分析物的偵測，具有快速、簡單、操作容易、高靈敏度和高選擇性等優點。

關鍵字

分散式液液微萃取法 ； 分散劑 ； 萃取劑 ； 基質輔助雷射脫游離 ； 飛行時間質譜儀

並列摘要

In this study, dispersive liquid-liquid microextraction method was employed for the extraction and preconcentration of digitoxin in an aqueous solution. The analyte was detected by the matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.
The appropriate mixture of 1 mL of dispersive solvent (tetrahydrofuran, THF) and 12 μL of extraction solvent (chloroform, CHCl3) was injected into a standard solution of digitoxin. After centrifugation, the extraction solvent was deposited on the bottom of the conical tube. The sediment phase was transferred and mixed with α-CHCA matrix before analyzing by a mass spectrometer.
The results of our experimental data for the determination of digitoxin showed the signal enhancement factor of this analyte could be as high as 1,200 after dispersive liquid-liquid microextraction. The limit of detection of digitoxin was 2.2 nM, the linear dynamic range was from 0.05 μM to 1 μM with a correlation coefficient (R2) of 0.9998, respectively and the relative standard deviation was within 10%.
The analytical method we proposed had also been successfully applied for the determination of digitoxin in biological fluids such as urine after simple pretreatment procedure. The advantages of this technique are fast, simple, easy sample preparation, high sensitivity and high selectivity.

並列關鍵字

dispersive liquid-liquid microextraction method ； dispersive solvent ； extraction solvent ； matrix-assisted laser desorption/ionization ； time-of-flight mass spectrometry