Page 110 - 理化检验-化学分册2025年第三期

周江平，等：氯甲酸异丁酯衍生结合气相色谱-质谱法测定葡萄酒和黄酒中7种生物胺的含量

Determination of 7 Biogenic Amines in Wine and Huangjiu by Gas
Chromatography-Mass Spectrometry Coupled with
Isobutyl Chloroformate Derivatization

ZHOU Jiangping , MU Yuxian , HE Chunying , ZHAI Jiangge , ZHAO Yongxin , WU Pinggu 2*
1
2
1
1
1
(1. Gucheng District Center for Disease Control and Prevention, Lijiang 674100, China;
2. Zhejiang Province Center for Disease Control and Prevention, Hangzhou 310051, China)
Abstract: At present, the method for the determination of biogenic amines in food in the national standard has cumbersome
operation and long detection time, and China has not yet developed a standard detection method for biogenic amines in wine.
Based on this, the title research was carried out. 100 μL of 50 mg · L −1 1,7-diaminoheptane (1,7-DAP) internal standard solution,
300 μL of saturated sodium bicarbonate solution and 0. 01 g of cross-linked polyvinylpyrrolidone (PVPP) were added into 1 mL
of wine or huangjiu samples, and the mixture was vortex purified for 5 min and centrifuged for 1 min. 0. 5 mL of supernatant
was taken, 70 μL of isobutyl chloroformate as the derivatizing agent was added, and the mixture was vortex reacted for 5 min at
room temperature. Then 100 μL of ethanol, and 150 μL of dichloromethane were added, and vortex extraction was performed
for 5 min. After centrifugation for 1 min, the lower dichloromethane extract was taken and dehydrated by anhydrous sodium
sulfate. 7 biogenic amines including 2-phenylethylamine (2-PEA), putrescine (PUT), cadaverine (CAD), histamine (HIS),
tryptamine (TRY), tyramine (TYR) and octopamine (OA) were determined by gas chromatography-mass spectrometry (GC-
MS). The derivatives of 7 biogenic amines were separated on DB-5MS capillary chromatographic column according to the column
temperature program, detected by electron impact ion source in selected ion monitoring mode, and quantified by internal standard
method. As shown by the results, the linear range of the standard curves of 7 biogenic amines was 0. 2-10. 0 mg · L −1 . Test for
−1
recovery at 3 concentration levels of 0. 5, 2. 0, 5. 0 mg · L was carried out on the actual samples, and the recoveries were in
the range of 83. 3%-116%. RSDs (n=6) of the determined values were less than 10%, and the lower limit of determination was
− 1
determined to be 0. 2 mg · kg . This method could fully meet the limit requirements of biogenic amines (HIS) in Australia and
other countries (2-10 mg · L −1 ).
Keywords: biogenic amine；gas chromatography-mass spectrometry (GC-MS)；histamine；wine； huangjiu

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