MOLECULES
·
2022
·Vol. 27
·期 4
·1318
·
IF 4.927
Jia Zheng,Zhanglan He,Kangzhuo Yang,Zhipeng Liu,Dong Zhao,Michael C. Qian
Wuliangye baijiu is one of the most famous Chinese liquors with a protected geographical indication. This study used LiChrolut®EN-based solid-phase extraction (SPE) and fractionation combined with comprehensive two-dimensional chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) to unveil its volatile composition. The volatiles were isolated with LiChrolut®EN-based SPE and traditional liquid-liquid extraction (LLE). The neutral/basic fractions from LLE and the SPE were fractionated on a LiChrolut®EN SPE column and analyzed by comprehensive GC×GC-TOFMS. Compared with LLE, more esters and alcohols were detected in the SPE-based extraction. The SPE fractionation and GC×GC-TOFMS analysis resulted in the identification of about 500 volatile compounds in more than 3000 peaks of the Wuliangye baijiu. The approach simplifies the complex baijiu composition into functional group-based fractions for reliable identification and analysis. This study provided a confidence volatile identification approach for Chinese baijiu based on the SPE fractionation GC×GC-TOFMS.Keywords:baijiu;volatile fractionation;Wuliangye;LiChrolut®EN SPE;GC×GC-TOFMS
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
MOLECULES
·
2021
·Vol. 26
·期 19
·6030
·
IF 4.412
Zhanglan He,Kangzhuo Yang,Zhipeng Liu,Mingzhe An,Zongwei Qiao,Dong Zhao,Jia Zheng,Michael C. Qian
Wuliangye baijiu is one of the most famous baijiu in China, with a rich, harmonic aroma profile highly appreciated by consumers. Thousands of volatiles have been identified for the unique aroma profile. Among them, fatty acid esters have been identified as the main contributors to the aroma profile. In addition, many non-ester minor compounds, many of which are more polar than the esters, have been identified to contribute to the characteristic aroma unique to Wuliangye baijiu. The analysis of these minor compounds has been challenging due to the dominance of esters in the sample. Thus, it is desirable to fractionate the aroma extract into subgroups based on functional group or polarity to simplify the analysis. This study attempts a new approach to achieve simultaneous volatile extraction and fractionation using tandem LiChrolut EN and silica gel solid-phase extraction (SPE) columns. A baijiu sample (10 mL, diluted in 40 mL of water) was first passed through the LiChrolut EN (1.0 g) column. The loaded LiChrolut EN column was then dried with air and coupled with a silica gel (5.0 g) SPE column with anhydrous Na2SO4(10.0 g) in between. The volatile compounds were eluted from the LiChrolut EN column and simultaneously fractionated on the silica gel column based on polarity. The simultaneous extraction and fractionation technique enabled the fractionations of all fatty acid esters into less polar fractions. Fatty acids, alcohols, pyrazines, furans, phenols, hydroxy esters, and other polar compounds were collected in more polar fractions. This technique was used to study the volatile compounds in Wuliangye, Moutai, and Fengjiu baijiu. In addition to fatty acid esters, many minor polar compounds, including 2,6-dimethylpyrazine, 2-ethyl-6-methylpyrazine, 2-ethyl-3,5-dimethylpyrazine,p-cresol, and 2-acetylpyrrole, were unequivocally identified in the samples. The procedure is fast and straightforward, with low solvent consumption.Keywords:Wuliangye baijiu;simultaneous extraction and fractionation;tandem SPE columns;fatty acid esters;polar compounds
研究领域:
食品科学
·
分析化学
·
风味化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2018
·
IF 3.52
Jia Zheng,Dong Zhao,Zhifu Peng,Kangzhuo Yang,Qiang Zhang,Yongkui Zhang
Changes of volatile compounds and sensory properties in the fermentation process of Wuliangye baobaoqu starter (WBS) were determined by sensory analysis, gas chromatography-olfactometry (GC/O) and GC quantitative analyses. The sensory properties of WBS changed from the sour, fruity, bready notes at the temperature-rise phase (3-day and 7-day) to the nutty and moldy notes at the temperature-fall phase (18-day, 21-day and 27-day). Acetic acid, methional, ethyl acetate, phenylethyl alcohol, ethyl 2-phenylacetate, 4-vinylguaiacol were potential aroma active compounds based on their Osme values. Results of GC quantitative analyses showed that the acids had the highest concentration. The concentration of ( E )-2-hexenal, ethyl acetate, isoamyl alcohol, phenylethyl alcohol, 2- n -pentylfuran, acetic acid and lactic acid increased with the fermentation time, presented the highest level in the temperature-rise phase and decreased after this period. The concentration of ( E,E )-2,4-hexadienal, 2,6-dimethylpyrazine, trimethylpyrazine, tetramethylpyrazine presented the highest level at the temperature-fall phase. Ethyl 3-methylbutanoate, ( E , E )-2,4-hexadienal, ( E , E )-2,4-nonadienal, acetic acid and butanoic acid had high odor active values. Results of principal component analysis showed that acetic acid, hexanal, ( E )-2-hexenal, lactic acid, isoamyl alcohol, 1-hexanol and 1-octen-3-ol were critical volatile chemicals to distinguish different WBS samples.
研究领域:
食品科学
·
分析化学
·
感官科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）