利用基質固相分散法結合微波衍生化以氣相層析質譜儀偵測醬油中3-單氯-1,2-丙二醇

Determination of 3-chloro-1, 2-propandiol in soy sauce by matrix solid phase dispersion combined with microwave derivation and GC-MS

張琬婷(Wan-ting Chang)

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(2008年)

摘要

3-單氯-1,2-丙二醇(3-chloro-1,2-propandiol)通常存在於含有蛋白水解產物的食物及調味料中。在醬油的製造過程，為了降低成本、增加產量，會用化學方法如以蛋白質與鹽酸反應取代發酵過程，而其中會有3-單氯-1,2-丙二醇的產生。3-單氯-1,2-丙二醇已被證實有致癌之可能性，但其傳統的偵測方法，不僅步驟繁瑣且費時。因此，建立一個省時而有效之分析方法是刻不容緩的。本研究主要利用基質固相分散法與固相微萃取技術，結合微波衍生化反應，以氣相層析質譜儀進行醬油中3-單氯-1,2-丙二醇之偵測。實驗中探討不同的衍生化試劑、微波衍生化條件、固相基質材質、沖堤溶劑的選擇及用量，與固相微萃取條件等參數，以尋求最佳條件來進行分析物之測定。實驗結果顯示此方法的最佳條件為:取18g的矽藻土與9ml樣品混合攪拌均勻，沖堤溶劑使用60mL的乙酸乙酯，真空濃縮定量後，加入200μL的HFBA衍生化試劑，經微波功率114 瓦照射加熱 8 分鐘，冷凝溫度為 5 ℃，進行衍生化反應。反應完成後以PA材質的固相微萃取纖維進行萃取，萃取時間為25分鐘，再注入GC-MS進行分析。偵測線性範圍在0.8~80μg/kg之間，迴歸係數在0.9946以上，相對標準偏差小於15.8％，偵測極限為0.2
μg/kg。結果顯示基質固相分散法結合微波衍生化以氣相層析質譜儀偵測醬油中3-單氯-1,2-丙二醇，為一快速、操作簡便、價格低廉，且具有良好再現性與靈敏度的新方法。

關鍵字

氣相層析質譜儀 ； 固相微萃取 ； 基質固相分散法 ； 醬油 ； 3-單氯-1 ； 2-丙二醇 ； 微波衍生化

並列摘要

Residual fatty acid esters (glycerol) present in the raw materials will undergo hydrolysis forming chloropropandiol. Amongst others, 1,3-dichloropropan-2-ol and 3-chloropropandiol are two of the most toxic chloropropanol found as contaminants in acid-hydrolysed vegetable protein (Acid-HVP), and a range of other foods and in gradients, most notably in soy sauce.
In general, determination of 3-MCPD in soy sauce is need a lot of pretreatment procedures, such as extraction by extrelut column, sonication, elution, concentration, derivation. It need a lot of toxic organic solvent, taking a longer time, and complicated procedures, will cause lost the recovery, error of determination.
The aim of this study is to develop an efficiency, fast, simple, analytical protocol that would provide valid analytical measurement in meeting the new action limits for 3-MCPD in soy sauce. In this study, a pretreatment combining with matrix solid-phase dispersion (MSPD) and microwave assisted derivation will been designed. Parameters which affect the sensitivity of determination such as MCPD conditions (the type of solid support, matrix modification, eluting solvent and sequence of addition), microwave conditions (irradiating power and time) were investigated, and solid-phase microextraction conditions (the type of fibres, extraction time, desorption time). From the experiment, it showed that the optimum MCPD conditions were obtained with diatomaceous earth of solid support, eluting solvent useing ethyl acetate for 60 ml and derivation reagent useing heptafluorobutyric acid (HFBA) for 200μl. Microwave conditions were obtained with irradiation power 114 Watt for 8 min. The linear ranges of the method were 0.8~80μg/kg with regression coefficient 0.9946. The proposed method is a simple, fast procedure for determining 3-MCPD from soy sauce.

並列關鍵字

Solid phase microextraction ； GC-MS ； Microwave assisted ； Matrix solid-phase dispersion ； Soy sauce ； 3-monochloro-1 ； 2-propandiol

參考文獻

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