臺灣博碩士論文加值系統

二甲基黃 (dimethyl yellow) 及二乙基黃 (diethyl yellow) 為人工合成而得之偶氮類色素 (azo dye)。二甲基黃已被國際癌症研究署 (International Agency for Research on Cancer, IARC) 列為 Group 2B，即為致癌物且具潛在危險性，會對人類和動物構成危險，職業工人長期接觸會造成接觸性皮膚炎，且會引起大鼠和小鼠的肝腫瘤及狗之膀胱腫瘤等。而二乙基黃無致突變性。
有鑑於 2014 年底我國爆發豆乾內非法摻入二甲基黃及二乙基黃之事件，此二色素之分析受到重視。本研究建立以高效能液相層析儀(high performance liquid chromatograph, HPLC) 搭配光電二極矩陣偵測器 (photodiode array detector, PDA) 分析食品之方法，包括探討 HPLC 之最適分析條件及樣品萃取之條件。
消泡劑以超音波輔助萃取效果優於微波輔助萃取，其二甲基黃及二乙基黃之回收率分別介於 87.9 98.9 及 86.8 94.4%；而使用微波輔助萃取時，二甲基黃及二乙基黃萃取回收率分別介於 93.3 97.1 及 92.5 95.4%。顯示使用超音波輔助萃取及微波輔助萃取法萃取，皆可有效萃取樣品中二甲基黃及二乙基黃。
B 牌咖哩粉以微波輔助萃取效果優於超音波輔助萃取，B 牌咖哩粉以超音波輔助萃取二甲基黃及二乙基黃萃取回收率分別介於 85.9 111.58 及 86.70 110.30%；而使用微波輔助萃取，二甲基黃及二乙基黃萃取回收率分別介於 86.5-96.39 及 87.3-92.14%。微波輔助萃取法萃取回收率範圍較窄，顯示使用微波輔助萃取之效果較佳。
以 HPLC-PDA 分析豆乾、消泡劑、咖哩粉等中之二甲基黃及二乙基黃，利用 Inertsil ODS-2 管柱搭配 2% 乙酸：乙腈：甲醇 = 15：20：65 (v/v/v) 為移動相，在波長 410 nm 下進行等位沖提，此方法二甲基黃及二乙基黃之偵測極限分別為 4.20 及 2.78 μg/kg，定量極限分別為 13.99 及 9.26 μg/kg，8 個樣品中，只有消泡劑被檢測出二甲基黃及二乙基黃，含量為 10.0 ± 0.1 及 9.7 ± 0.2 μg/g。

Dimethyl yellow (DMY) and diethyl yellow (DEY) are artificial azo dyes. DMY has been classified as a Group 2B carcinogen by the IARC (International Agency for Research on Cancer). It is potentially harmful to human and animals. People who contacts with it for extended period of time may suffer from dermatitis. DMY has been proved to cause hepatic cancer (HCC) in rats and mice. It also causes urologic cancer in canines. DEY has no record about mutagen characteristics.
DMY and DEY was found in domestic bean curd products in 2014. Since then, methods for detection of these illegal substances has attracted public attention. This research is to explore an optimal procedure to determine these two azo dyes in food products by using a high performance liquid chromatograph (HPLC) along with a photodiode array (PDA) detector.
Ultrasonic-assisted extraction (UAE) method was found to have better result for extracting both DMY and DEY from a defoamer sample than microwave-assisted extraction (MAE) method. For the UAE method, the recoveries for DMY and DEY were 87.9 98.9% and 86.8 94.4% respectively. For the MAE method, the recoveries for DMY and DEY were 93.3 97.1% and 92.5 95.4% respectively. The results showed that both UAE and MAE were proved to be effective in DMY and DEY extraction.
For brand B curry powder, MAE method had better results than UAE method. The recoveries of DMY and DEY for MAE method were 85.9 111.58% and 86.70 110.30%, respectively, while the recoveries of DMY and DEY for UAE method were 86.5-96.39% and 87.3-92.14%, respectively. MAE method had narrower recovery range, which suggest the better result.
HPLC-PDA was used to determine both DMY and DEY contents in bean curds, defoamers, curry powder, and other samples. An Inertsil ODS-2 column was used for separation. The detection wavelength was set at 410 nm. The mobile phase was 2% acetic acid in water：acetonitrile：methanol = 15：20：65 (v/v/v). The limits of detection of DMY and DEY were 4.20 and 2.78 μg/kg, respectively, and the limits of quantitation of DMY and DEY were 13.99 and 9.26 μg/kg, respectively. Of the 8 samples, only the defoamer was detected to contain DMY and DEY. Their contents were 10.0 ± 0.1 and 9.7 ± 0.2 μg/g, respectively.

摘要 I
Abstract II
目錄 III
圖目錄 V
表目錄 VII
壹、前言 1
貳、文獻整理 2
一、色素之種類及作用 2
二、二甲基黃 2
三、二乙基黃 3
四、有關二甲基黃及二乙基黃應用於食品之法規 3
五、國內外食品中摻入二甲基黃及二乙基黃之事件 3
六、食品中二甲基黃及二乙基黃之測定 4
(一) 樣品前處理之方法 4
(二) 分析方法 5
參、材料與方法 8
一、實驗材料 8
(一) 樣品 8
(二) 標準品 8
(三) 藥品 8
(四) 層析管柱 8
(五) 儀器設備 8
二、實驗流程 10
三、實驗方法 11
(一) 建立 HPLC 分析二甲基黃及二乙基黃之方法 11
(二) 二甲基黃及二乙基黃之萃取 11
(三) 偵測極限、定量極限及回收率之測定 12
肆、結果與討論 14
一、以 HPLC 分析二甲基黃及二乙基黃之條件 14
(一) 吸收波長 14
(二) 移動相 14
(三) 檢量線 14
(四) 最低偵測極限及定量極限 14
二、以不同方式萃取豆乾消泡劑中二甲基黃及二乙基黃之含量 15
(一) 超音波輔助萃取 (Ultrasonic-assisted extraction, UAE) 15
(二) 微波輔助萃取 (Microwave-assisted extraction, MAE) 15
三、市售食品中二甲基黃和二乙基黃之檢測 15
四、回收率試驗 16
伍、結論 18
陸、參考文獻 19
柒、圖表 23
捌、附錄 51

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