酒精性飲料中胺基甲酸乙酯之檢驗方式之探討及建立

Investigation and Establishment on the Test Method for Ethyl Carbamate in Alcoholic Beverages

蔡雯茹(Wen-Ju Tsai)；張美華(Mei-Hua Chang)；曾素香(Su-Hsiang Tseng)；高雅敏(Ya-Min Kao)；周秀冠(Hsiu-Kuan Chou)；陳惠芳(Hwei-Fang Cheng)

酒精性飲料 ； 胺基甲酸乙酯 ； 氣相層析串聯質譜儀 ； alcoholic beverages ； ethyl carbamate ； gas chromatograph/tandem mass spectrometer

食品藥物研究年報

6期（2015 / 12 / 01）

1 - 9

繁體中文

胺基甲酸乙酯(ethyl carbamate)為發酵過程中自然產生之物質，廣泛存在於發酵食品及發酵飲料中，因可能具有致癌性而被各國所關注。各國針對不同種類的酒訂立不同之限量標準，規範為15-1000 ng/mL，其中法國針對水果白蘭地訂定限量標準1000 ng/mL。酒類檢體添加同位素內部標準品(20 ng/mL)載入矽藻土固相萃取匣進行液/液分配萃取，以正戊烷沖洗及乙醚沖提後，檢液以氣相層析串聯質譜儀(GC/MS/MS)配合多重反應偵測(MRM)模式偵測，以內部標準品法進行定量。選取葡萄酒、清酒、白蘭地、高粱及啤酒進行添加回收試驗，於檢體添加標準溶液使每毫升檢體含有10、50及100 ng胺基甲酸乙酯，同日間平均回收率介於87.6-113.0%，變異係數為0.4-8.0%，異日間所得之平均回收率介於90.9-108.1%，變異係數為0.4-10.2%，本檢驗方法之定量極限為10 ng/mL。以建立之方法進行市售31件酒品之檢驗，穀類釀造酒類9件的胺基甲酸乙酯濃度範圍為未檢出-1720 ng/mL，其中有3件濃度超出1000ng/mL，水果釀造酒類6件為未檢出-48 ng/mL，啤酒類3件為未檢出，再製酒類2件為43-124 ng/mL，蒸餾酒類11件為未檢出-92 ng/mL，檢驗結果已提供相關管理單位參考。

Ethyl carbamate (EC) was found as a natural constituent in many fermented foods and alcoholic beverages. The international community concerned about the carcinogenic potential of EC to humans. Hence, numerous countries has established their own maximum allowed levels of EC in various alcoholic beverages from 15 to 1000 ng/mL, such as, France had set not more than 1000 ng/mL in fruit brandy. In this study, each sample of alcoholic beverages was added of internal standard (20 ng/mL) and then loaded into diatomaceous earth cartridge. The cartridge was rinsed with pentane then eluted by diethyl ether. The extract was analyzed by the gas chromatograph/tandem mass spectrometer (GC/MS/MS) with multiple reaction monitoring (MRM) mode. The quantification was done by internal standard method. Samples of wine, sake, brandy, spirits, and beer (1 mL) were fertilized with different levels of EC, including 10, 50 and 100 ng for recovery studies. The intraday average recoveries of alcohol beverages were from 87.6 to 113.0% with the coefficients of variation (CVs) between 0.4 and 8.0%. The interday average recoveries ranged from 90.9 to 108.1% with the CVs between 0.4 and 10.2%. The limit of quantification was estimated as 10 ng/mL for this method. The established method was applied for survey of 31 alcoholic beverages from retail stores. The results showed the EC in 9 grain brewed beverages, 6 fruit wines, 2 reprocessed wines and 11 spirits were from not detected to 1720, 48, 124 and 92 ng/mL, respectively. 3 beers were not detected. Amount 9 grain brewed beverages, 3 of them were above 1000 ng/mL. The survey reports had provided to authorities for references.