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采用分散液液微萃取-气相色谱-质谱联用技术测定红参制品中的乙二醛、甲基乙二醛和双乙酰。

Determination of glyoxal, methylglyoxal, and diacetyl in red ginseng products using dispersive liquid-liquid microextraction coupled with GC-MS.

机构信息

Korea Food Research Institute, Jeollabuk-do, Republic of Korea.

Department of Environmental Toxicology, University of California, Davis, CA, USA.

出版信息

J Sep Sci. 2019 Mar;42(6):1230-1239. doi: 10.1002/jssc.201800841. Epub 2019 Feb 7.

Abstract

A simple and rapid dispersive liquid-liquid microextraction method coupled with gas chromatography and mass spectrometry was applied for the determination of glyoxal as quinoxaline, methylglyoxal as 2-methylquinoxaline, and diacetyl as 2,3-dimethylquinoxaline in red ginseng products. The performance of the proposed method was evaluated under optimum extraction conditions (extraction solvent: chloroform 100 μL, disperser solvent: methanol 200 μL, derivatizing agent concentration: 5 g/L, reaction time: 1 h, and no addition of salt). The limit of detection and limit of quantitation were 1.30 and 4.33 μg/L for glyoxal, 1.86 and 6.20 μg/L for methylglyoxal, and 1.45 and 4.82 μg/L for diacetyl. The intra- and interday relative standard deviations were <4.95 and 5.80%, respectively. The relative recoveries were 92.4-103.9% in red ginseng concentrate and 99.4-110.7% in juice samples. Red ginseng concentrates were found to contain 191-4274 μg/kg of glyoxal, 1336-4798 μg/kg of methylglyoxal, and 0-830 μg/kg of diacetyl, whereas for red ginseng juices, the respective concentrations were 72-865, 69-3613, and 6-344 μg/L.

摘要

一种简单快速的分散液液微萃取方法与气相色谱-质谱联用,用于红参制品中乙二醛(作为喹喔啉)、甲基乙二醛(作为 2-甲基喹喔啉)和双乙酰(作为 2,3-二甲基喹喔啉)的测定。在最佳萃取条件下(萃取溶剂:100 μL 氯仿,分散溶剂:200 μL 甲醇,衍生剂浓度:5 g/L,反应时间:1 h,不加盐)评价了所提出方法的性能。乙二醛的检出限和定量限分别为 1.30 和 4.33 μg/L,甲基乙二醛为 1.86 和 6.20 μg/L,双乙酰为 1.45 和 4.82 μg/L。日内和日间相对标准偏差分别<4.95 和 5.80%。在红参浓缩物和果汁样品中的相对回收率分别为 92.4-103.9%和 99.4-110.7%。红参浓缩物中乙二醛含量为 191-4274 μg/kg,甲基乙二醛含量为 1336-4798 μg/kg,双乙酰含量为 0-830 μg/kg;而红参果汁中乙二醛、甲基乙二醛和双乙酰的浓度分别为 72-865、69-3613 和 6-344 μg/L。

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