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采用4-(2,3-二甲基-6-喹喔啉基)-1,2-苯二胺作为衍生试剂的柱前衍生化-高效液相色谱-紫外检测法测定啤酒中的双乙酰

Determination of Diacetyl in Beer by a Precolumn Derivatization-HPLC-UV Method Using 4-(2,3-Dimethyl-6-quinoxalinyl)-1,2-benzenediamine as a Derivatizing Reagent.

作者信息

Wang Ji-Yu, Wang Xin-Jie, Hui Xian, Hua Shui-Hong, Li Heng, Gao Wen-Yun

机构信息

National Engineering Research Center for Miniaturized Detection Systems and College of Life Sciences, Northwest University , 229 North Taibai Road, Xi'an, Shaanxi 710069, China.

出版信息

J Agric Food Chem. 2017 Mar 29;65(12):2635-2641. doi: 10.1021/acs.jafc.7b00990. Epub 2017 Mar 21.

Abstract

Diacetyl is an important flavoring compound in many foods, especially in beer. In the present study, we developed and validated a new precolumn derivatization HPLC-UV method for the determination of diacetyl using 4-(2,3-dimethyl-6-quinoxalinyl)-1,2-benzenediamine as a novel derivatizing reagent. After derivatization with the reagent at a pH value 4.0 at ambient temperature for 10 min, diacetyl was analyzed on an ODS column and detected at 254 nm. The results show that the correlation coefficient of the method is 0.9991 in the range of 0.10 to 100.0 μM diacetyl, and the limit of detection is 0.02 μM. The method was further evaluated in the analysis of beer samples with the recoveries ranging from 94.4 to 102.6% and RSDs from 1.36 to 3.33%. The concentrations of diacetyl in 8 beer samples were determined in the range of 0.19 to 0.42 μM. The method established in this study may be well suitable for the determination of diacetyl in beer.

摘要

双乙酰是许多食品尤其是啤酒中的一种重要调味化合物。在本研究中,我们开发并验证了一种新的柱前衍生化高效液相色谱 - 紫外检测法,用于测定双乙酰,该方法使用4-(2,3 - 二甲基 - 6 - 喹喔啉基)-1,2 - 苯二胺作为新型衍生试剂。在室温下,用该试剂在pH值为4.0的条件下衍生化10分钟后,在ODS柱上分析双乙酰,并在254 nm处进行检测。结果表明,该方法在双乙酰浓度为0.10至100.0 μM范围内的相关系数为0.9991,检测限为0.02 μM。该方法在啤酒样品分析中得到进一步评估,回收率在94.4%至102.6%之间,相对标准偏差在1.36%至3.33%之间。测定了8个啤酒样品中双乙酰的浓度,范围在0.19至0.42 μM之间。本研究建立的方法可能非常适合啤酒中双乙酰的测定。

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