以固相微萃取結合氣相層析法快速偵測賽滅淨農藥之研究

A Study of Rapid Analysis for Cyromazine by the Solid-phase Microextraction / Gas Chromatography

溫洪能(Hong-Neng Wun)

指導教授 ： 許道平

淡江大學/工學院/水資源及環境工程學系碩士班/碩士(2005年)

https://doi.org/10.6846/TKU.2005.00691

摘要

本研究之目的為經簡單處理之蔬果樣品，結合固相微萃取與氣相層析儀偵測樣品(包心葉菜類、小葉菜類、蕃茄)中賽滅淨之含量。透過直接萃取樣品再置入儀器進行分析不但能有效縮短分析時間，且能有效降低偵測極限。
農藥賽滅淨被歸類為殺蟲劑，其代謝產物蜜胺引發癌症之疑慮，偵測賽滅淨之方法包含液相層析/紫外光偵檢器以及氣相層析儀/火焰離子偵檢器，當樣品送入儀器前，必須經過適當前處理，樣品萃取前處理經常使用大量有機溶劑，處理過程更是耗時繁瑣，分析效率實不經濟，如果能將實驗分析時間有效縮短，則有助於實驗效率之提升。
經直交表實驗設計尋求最佳實驗條件，進而探討此研究方法之可行性與實際樣品分析之應用，本研究以直交表L27(38)實驗設計所得最佳實驗條件如下，萃取時間30min，萃取溫度50℃，脫附時間5min，脫附溫度250℃，攪拌速率1000rpm，pH=7，樣品體積4mL。在此操作條件下，線性範圍0~15μg/mL，最佳回歸係數0.9932，方法偵測極限0.015μg/mL，之平均回收率105.68%(添加濃度0.2~1μg/mL, n=3)，相對標準偏差8.79%(n=7)。另採得真實蔬果樣品於淡水黃昏市場蔬果種類有包心菜類、小葉菜類、蕃茄(聖女品種)等三種樣品。偵測結果顯示，在蕃茄樣品發現賽滅淨農藥含量為194μg/g，且經過30天後(儲存冰箱冷藏4℃)，蔬果樣品內賽滅淨農藥由194μg/g降解為41μg/g。

關鍵字

賽滅淨 ； 固相微萃取 ； 實驗設計 ； 直交表 ； 蕃茄

並列摘要

The aim of this study is to use solid phase microextraction (SPME) technique combined with gas chromatography (GC) applied to determine the cyromazine residues in food samples. In this study, the fiber in SPME coated with 85μm Polyacrylate(PA) was used to extract cryomazine in direct immerse(DI) extraction model. The direct use of SPME to extract an aqueous suspension of solid samples has been studied. The extraction parameters for optimization have also been investigated by the design of experiment method.
Cyromazine (N-cyclopropyl-1,3,5-triazine-2,4,6-triamine) is a triazine pesticide used for fly control in cattle manure, field crops, vegetables and fruits by inhibiting insect growth. The cyromazine can be hydrolysed at extreme pH or photodegraded leading to the stable heterocyclic structure melamine (1, 3,5-triazine-2,4,6-triamine).
The design of experiment (DOE) method was applied initially to use a minimum number of experiments. Orthogonal array techniques are used to investigate the simultaneous variation of several parameters and the investigation of interactions between parameters. In order to estimate the optimum levels and determine the relative magnitude of the effect of various factors. the total 27 experiments were completed. Finally, the extraction parameters of SPME-GC for optimization were as follows：adsorption time 30min；adsorption temperature 50℃；desorption time 5min；desorption temperature 250℃；stirring rate 1000rpm；pH=7；sample volume 4mL. The limit of method detection was 0.015μg/mL. and the relative standard deviation was 8.79%(n=7). It is found that the cyromazine concentration in tomatoes from local market was 194μg/g. and the Recoveries were 105.68 %( concentration range for standard addition, 0.2~1.0μg/mL, n=3). The regression coefficient and linear range of the calibration curve were 0.9932, 0~15μg/mL, respectively.

並列關鍵字

Cyromazine ； solid-phase microextraction (SPME) ； design of experiment (DOE) ； Orthogonal array (OA) ； Tomato

參考文獻

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