以微波輔助頂空液相微萃取技術結合氣相層析質譜儀偵測柑橘中農藥之殘留

Determination of pesticides in orange fruits by microwave assisted headspace liquid phase microextraction and GC-MS

邱耀賢(Chiou-yau shian)

指導教授 ： 魏銘琪

中臺科技大學/健康科學院/食品科技研究所/碩士(2009年)

https://doi.org/10.6822/CTUST.2009.00016

摘要

摘要
本研究利用微波頂空液相微萃取法結合氣相層析質譜儀，對柑橘類水果中Fenthion(芬殺松)、Bromopropylate(新殺螨)、Fenitrothion(撲滅松)等農藥殘留進行分析與偵測。實驗中，在樣品內分析物經由微波快速加熱後，隨著水蒸氣汽化至氣相中，藉由擴散作用進入頂空位置的中空纖維管，為纖維內萃取溶劑所吸附，同時達到萃取及濃縮的效果。Fenthion(芬殺松)、Bromopropylate(新殺螨)、Fenitroth(撲滅松)樣品經萃取後，將萃取溶劑抽取定量直接注入氣相層析儀質譜儀進行偵測與分離。為建立本偵測方法最佳化條件，實驗中分別對影響分析物萃取的參數進行探討，其參數有溶劑種類，萃取中空纖維管的長度，微波照射時間，冷凝系統溫度，微波功率與時間，鹽析效應，樣品溶液之pH值。實驗結果顯示微波頂空液相微萃取之最佳化條件為萃取溶劑使用1-Octanol、中空纖維管長度1.5cm、微波照射時間10分鐘、微波功率167W、冷凝系統溫度25℃，添加NaCl 0.1%及樣品溶液之pH值為4。在最佳的條件下進行待測物之分析，線性偵測範圍為Fenthion(0.1~10μg/l)、Fenitrothion(0.1~10μg/l)、Bromopropylate (1~100μg/l)，偵測極限Fenthion (0.0153μg/l)、Fenitrothion (0.02μg/l)、Bromopropylate (0.03μg/l)，將此方法應用在偵測柳丁真實樣品偵測到含有Fenthion (0.1μg/l)，回收率介於77~93%。研究結果顯示微波輔助頂空液相微萃取技術結合氣相層析儀對偵測柑橘類農藥殘留，為一操作簡便、價格低廉、快速、不受基質干擾、且只需使用極微量有機溶劑同時此方法亦皆有良好的再現性與靈敏度。

關鍵字

芬殺松 ； 撲滅松 ； 新殺螨 ； 微波輔助 ； 中空纖維液相微萃取 ； 頂空

並列摘要

The purpose of this study is to detect Fenthion、Brompropylat and Fenitrothion in orange fruits by developing the technique of sample pretreatment, microwave assisted headspace hollow fiber liquid-phase microextraction (MA-HS-HF-LPME).
The analytes in aqueous matrix are extracted to organic solvent in the fiber of liquid-phase microextraction in the headspace with the aid of microwave irradiation; thus, the analytes in orange fruits matrix were firstly extracted into the aqueous solution and then followed the same procedures in aqueous matrix. After the compounds were collected, the extract was injected in GC injection port and analyzed by GC-MS. Parameters affecting the extraction efficiency such as selections of solvents, length of hollow fiber, pH in the solution addition of salt to sample solution, temperature of cooling water, the power and irradiation time of microwave as well as the time of extraction were investigated. The optimum extraction efficiency of pesticides in aqueous matrix was obtained by using octanol as extract solvent and the sample solution at pH 4 with irradiation power 167 watts for 10 minutes. The detection limits varied from Fenthion (0.02μg/l) Fenitrothion (0.02μg/l) Bromopropylate(0.03μg/l). In a real sample (orange fruits), we detected Fenthion with 0.1 μg/L. The recovery of real sample were between 77-93%. The proposed method is a simple, fast, and trace organic solvent procedure for determing pesticides from complicated sample matrix.

並列關鍵字

Microwave assisted ； Liquid phase microextraction ； Headspace ； Fenthion ； Bromopropylate ； Fenitrothion

參考文獻

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