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研究生:林書勳
研究生(外文):Shu-Shiun Lin
論文名稱:偽造金門高粱酒鑑識方法之研究:揮發性成分分析
論文名稱(外文):Identification of Counterfeit Kimen Kaoliang Liquor: Analysis of Volatile Compounds
指導教授:張維敦張維敦引用關係
指導教授(外文):Wei-Tun Chang
學位類別:碩士
校院名稱:中央警察大學
系所名稱:鑑識科學研究所
學門:軍警國防安全學門
學類:警政學類
論文種類:學術論文
論文出版年:2012
畢業學年度:100
語文別:中文
論文頁數:121
中文關鍵詞:偽造金門高梁酒電子鼻氣相層析穩定同位素比值譜儀氣相層析質譜儀主成分分析
外文關鍵詞:counterfeit Kimmen Kaoliang Liquorelectronic-nose(E-Nose)gas chromatography-mass spectrometry (GC-MS)gas chromatography- stable isotope ratio mass spectrometry(GC-IRMS)principle component analysis(PCA)
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自從政府開放民間製酒,有些業者為降低生產成本,賺取價差,因
而開始製造販賣偽造酒品以謀取暴利。偽造酒品問題日益嚴重,在財政部國
庫署公佈的查獲案件當中,金門高粱酒為常見之被仿冒酒種。因此,研發快
速鑑別金門高粱真偽之技術著實有其必要性。
本研究使用電子鼻、氣相層析質譜法以及氣相層析穩定同位素比質譜法,
針對金門高粱酒、國內常見品牌之高梁酒以及偽造金門高粱酒進行揮發性成
分之分析。樣品前處理是選用固相微萃取法吸附高粱酒樣本之揮發性成分,
並依吸附溫度、吸附時間及脫附時間進行調整,選訂出最佳萃取條件。經電
子鼻及氣相層析質譜法分析所得層析圖之各個滯留時間視為一個感應器,匯
入Alpha Soft 統計軟體進行PCA 分析。氣相層析同位素比質譜法分析後,
選取9 種揮發性成分,計算各個成分其δ13C 之平均值與標準差。結果顯示,
電子鼻及氣相層析質譜法結合PCA,以人工選取金門高粱酒特異波峰模進行
分析,均能區分金門高粱酒與非金門高粱酒。金門高粱酒樣本經氣相層析穩
定同位素比值譜法分析後,建立9 種揮發性成分其δ13C 之變異範圍,將8
種非金門高粱酒樣本與金門高粱酒樣本進行比對,7 種樣本有明顯差異,1
種樣本差異較小。
經氣相層析質譜法分析後,發現金門高粱酒含有兩種獨特揮發性成分,
分別為Creosol 與p-Ethylguaiacol,針對此2 種化合物之含量與內標準品之含
量比值,推估偽造金門高粱酒中所含金門高粱酒百分比。T1 樣本被估算約
含10.9%~20.6%金門高粱酒,T2 樣本約含3.7%~4.1%金門高粱酒。
Since the government liberalized private distilleries, some of manufacturers
began to make counterfeit spirits in order to reduce production cost and reap huge
profit. Counterfeit spirits have become a growing problem in our society. In the
seized cases published by the National Treasury Agency , Kimmen Kaoliang
Liquor is shown as one of the common counterfeit wines in Taiwan. Therefore, the
development of the rapid and accurate methods for the identification of counterfeit
Kimmen Kaoliang Liquor is anxious demand.
The study herein is focused on the analysis of volatile compounds in Kimmen
Kaoliang Liquor, commercial sorghum spirits and counterfeit Kimmen Kaoliang
Liquor by using electronic-nose approach(E-Nose), gas chromatography-mass
spectrometry(GC-MS) and gas chromatography- stable isotope ratio mass
spectrometry(GC-IRMS). Sample pretreatment is performed by using headspace -
solid phase microextraction(HS-SPME) to adsorb volatile compounds in spirit
samples. Extraction conditions such as extraction time, temperature and desorption
time are optimized based on the evaluation of different parameters. The peaks
selected as sensors from E-Nose and GC-MS are further analyzed by principle
component analysis(PCA). In the GC-IRMS analysis, nine volatile compounds
were selected and their δ13C values are individually calculated.
The results indicate that Kimmen Kaoliang Liquor can be discriminated from
other sorghum spirits samples by PCA approach. The resulting data from GCIRMS
show that seven kinds of sorghum spirit samples were significantly
different from Kimmen Kaoliang Liquor samples in eight kinds of sorghum spirit
samples. Only one sample shows slightly different.
According to comparisons among all samples, two specific volatile compounds,
Creosol and p-Ethylguaiacolin, are found in Kimmen Kaoliang Liquor. The
intensity ratio of these two volatile compounds using an internal standard is
adopted to estimate the content of Kimmen Kaoliang Liquor in counterfeit
Kimmen Kaoliang Liquor samples. The results estimate that there are 10.9%
~20.6% Kimmen Kaoliang Liquor in T1 counterfeit sample and 3.7%~4.1% in
counterfeit T4 sample.
圖目錄………………………………………………………………………………………………III
表目錄……………………………………………………………………………...……………….IV
第一章 緒論…………………………………………………………………………........................1
1-1 研究動機與目的………………………………………………………………………………1
1-2 違法酒類之種類………………………………………………………………………………3
1-2-1 私酒……………………………………………………………………………………….3
1-2-2 劣酒……………………………………………………………………………………….3
1-2-3 仿冒酒…………………………………………………………………………………….4
1-3 氣相層析質譜儀………………………………………………………………………………4
1-4 電子鼻之原理與應用………………..………………………………………………………..5
1-5 固相微萃取法…………………………………………………………………………………7
1-6 自然界穩定同位素的分化作用及植物的碳循環…………………………………………..10
1-7 氣相層析穩定同位素質譜法…………...…………………………………………………...12
1-8 穩定同位素比值於刑事鑑識之應用………………………………………………………..15
1-9 酒類中的碳穩定同位素比值………………………………………………………………..16
第二章 GC-Flash 型電子鼻應用在金門高粱酒與市售高粱酒及偽造金門高粱酒揮發性成分之
比較………………………………………………………………………………………19
2-1 前言…………………………………………………………………………………………..19
2-2 實驗材料與方法……………………………………………………………………………..20
2-2-1 高粱酒類樣品…………………………………………………………………………...20
2-2-2 實驗設備………………………………………………………………………………...21
2-2-3 頂空固相微萃取法前處理……………………………………………………………...21
2-2-4 GC-Flash 型電子鼻分析………………………………………………………………..23
2-2-5 主成分分析…………………..…………………………………………………………23
2-3 結果與討論…………………………………………………………………………………..25
2-3-1 頂空固相微萃取法最適化條件之選定……………………………………………….25
2-3-2 金門高粱酒與市售高粱酒及偽造金門高粱酒揮發性成分之比較…………………...25
第三章 氣相層析質譜法應用在金門高粱酒與市售高粱酒及偽造金門高粱酒揮發性成分之比
較…………………………………………………………………………………………31
3-1 前言…………………………………………………………………………………………..31
3-2 實驗材料與方法……………………………………………………………………………..32
3-2-1 高粱酒類樣品…………………………………………………………………………...32
3-2-2 實驗設備………………………………………………………………………………...32
3-2-3 頂空固相微萃取法前處理……………………………………………………………...32
3-2-4 氣相層析質譜法之分析………...………………………………………………………33
3-2-5 主成分分析…………………..………………………………………………………….33
3-3 結果與討論…………………………………………………………………………………..34
3-3-1 金門高粱酒與市售高粱酒及偽造金門高粱酒揮發性成分比較……………………...34
第四章 氣相層析質譜法應用在偽造酒品調兌比例之分析……………………………………42
4-1 前言…………………………………………………………………………………………..42
4-2 實驗材料與方法……………………………………………………………………………..43
4-2-1 高粱酒類樣品…………………………………………………………………………...43
4-2-2 實驗藥品………………………………………………………………………………...44
4-2-3 實驗設備………………………………………………………………………………...44
4-2-4 頂空固相微萃取法前處理……………………………………………………………...44
4-2-5 氣相層析質譜法之分析………………………………………………………………...45
4-2-6 內標準法之相對含量分析……………………………………………………………...46
4-2-7 建立檢量線……………………………………………………………………………...46
4-3 結果與討論…………………………………………………………………………………..48
4-3-1 金門高粱酒獨特揮發性成分含量百分比分析……………………...............................48
4-3-2 偽造金門高粱酒調兌比例之估算……………………………………………………...49
第五章 氣相層析穩定同位素比質譜法應用在金門高粱酒與市售高粱酒及偽造假酒之碳同位
素比值分析………………………………………………………………………………53
5-1 前言…………………………………………………………………………………………..53
5-2 實驗材料與方法……………………………………………………………………………..54
5-2-1 高粱酒類樣品…………………………………………………………………………...54
5-2-2 實驗設備………………………………………………………………………………...54
5-2-3 頂空固相微萃取法前處理……………………………………………………………...55
5-2-4 氣相層析穩定同位素比質譜法分之析………………………………………………...55
5-3 結果與討論…………………………………………………………………………………..58
5-3-1 金門高粱酒之δ13C 分析…………………….................................................................58
5-3-2 58 金門高粱酒與他牌高粱酒之δ13C 分析比較………………………………………59
5-3-3 58 金門高粱酒與偽造金門高粱酒之δ13C 分析比較…………………………………59
5-3-4 38 金門高粱酒與偽造金門高粱酒之δ13C 分析比較…………………………………59
5-3-5 結論……………………………………………………………………………………...59
第六章 結論與建議………………………………………………………………………………70
參考文獻……………………………………………………………………………………………72
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