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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2025 · IF 2.8

Comparison of three extraction methods, DMU-SPME, SAFE, and SDE, for the analysis of flavor compounds in soy sauce

Yun-Jiao Ma,An-Qi Bi,Ping Li,Bei-Wei Zhu,Ming Du,Xian-Bing Xu

The dual mode unity solid-phase microextraction (DMU-SPME) was evaluated against traditional solvent-based methods, including solvent-assisted flavor evaporation (SAFE) and simultaneous distillation extraction (SDE), to explore its potential as an alternative. Compared to SAFE and SDE, DMU-SPME is a green extraction technology for volatile organic compounds. The results demonstrated that DMU-SPME significantly outperformed both SAFE and SDE in extracting medium-volatility compounds (retention time of 20–40 min), identifying 55 unique volatiles. With the exception of hydrocarbons, DMU-SPME exhibited superior extraction efficiency and significantly better stability compared to both SAFE and SDE methods. Thus, DMU-SPME proves to be a promising alternative for the comprehensive extraction of volatile organic compounds.

研究领域: 食品科学 · 分析化学
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Food Analytical Methods · 2017 ·Vol. 11 ·期 2 ·343-354 · IF 2.038

Comparison of Four Extraction Methods, SPME, DHS, SAFE, Versus SDE, for the Analysis of Flavor Compounds in Natto

Liu Ye,Su Hang,Song Huan-Lu

Natto is a kind of traditional fermentation food. Organic soybean of china northeast was selected as the material to produce natto according to the condition optimized before. Four extraction methods (SAFE (solvent-assisted flavor evaporation), SDE (simultaneous distillation and extraction), SPME (solid phase microextraction), and DHS (dynamic headspace sampling)) were applied to extract the volatile compounds of natto. Aroma compounds were separated and analyzed with gas chromatography-olfactometry-mass spectrometry (GC-MS/O) of DB-5 and DB-Wax capillary columns. Seventy-seven compounds were identified by four extraction methods. Among them, 42, 23, 31, and 36 compounds were identified by SPME, DHS, SDE, and SAFE, respectively. SAFE and SDE had a better extraction effect on ester, ether, and aromatic compounds, while SPME and DHS could extract ketone, acid, and pyrazine compounds effectively. SPME was fit for the extraction of natto aroma compounds. These compounds included 14 ketones, 9 alcohols, 4 aldehydes, 6 acids, 4 sulfur compounds, 5 esters, 8 pyrazines, 19 aromatics, and 8 others. Fourteen compounds were identified as key aroma compounds in natto, including 2,3-butanedione, 5-methyl-2-hexanone, 3-hydroxy-2-butanone, 2-nonanone, furaldehyde, acetic acid, 2-ethyl butyric acid, ethyl acetate, 2,5-dimethylpyrazine, 2,3,5-trimethylpyrazine, 3,5-dimethyl-2-ethylpyrazine, 2,3,5,6-tetramethylpyrazine, 2,3,5-methyl-6-ethylpyrazine, and benzaldehyde. Pyrazine was the important aroma compound with the high FD (flavor dilution) value in natto.

研究领域: 食品科学 · 分析化学
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Food Analytical Methods · 2016 ·Vol. 10 ·期 4 ·931-942 · IF 2.167

Reducing the Influence of the Thermally Induced Reactions on the Determination of Aroma-Active Compounds in Soy Sauce Using SDE and GC-MS/O

Feng Yunzi,Cai Yu,Sun-Waterhouse Dongxiao,Fu Xiong,Su Guowan,Zhao Mouming

A method based on simultaneous distillation extraction (SDE) coupled with gas chromatography–mass spectrometry/olfactometry (GC-MS/O) was developed for the analysis of volatile profiles in soy sauce. Its optimum operating conditions were as follows: 100 mL soy sauce plus 100 mL saturated brine; 2 h extraction using 50 mL dichloromethane. Eighty-eight volatile compounds were identified. Of these, 26 aroma-active compounds were detected by GC-O including 3-(methylthio)propanal, 2-methoxy-4-vinylphenol, 2-methoxyphenol, 2-methylbutanoic acid, 2,3-butanedione, phenylacetaldehyde, 2-ethyl-6-methylpyrazine, 3-methylbutanal, 2-methylbutanal, 3-methyl-1-butanol, and 2-methyl-1-butanol (which occurred at a high odor intensity in both high-salt liquid-state fermentation soy sauce (HLFSS) and low-salt solid-state fermentation soy sauce (LSFSS). SDE analysis of the odorless soy sauce indicated 12 volatiles (mainly Strecker aldehydes and α-dicarbonyl compounds). Thus, the proportions of these compounds (1.94–54.07 %) shown in previous GC-MS results could result from thermal degradation of non-volatile compounds in soy sauce. Especially, the contribution of 3-methylbutanal, 2-methylbutanal, phenylacetaldehyde, 3-(methylthio)propanal, and 2,3-butanedione to the aroma of soy sauce could be overestimated by conventional SDE-GC-O. With a full consideration of such limitations, this study will improve the application of SDE on aroma analysis of complex food matrix.

研究领域: 食品科学 · 分析化学
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Food Analytical Methods · 2015 ·Vol. 9 ·期 5 ·1188-1198 · IF 1.956

Characterization of Aroma-Active Compounds of Pu-erh Tea by Headspace Solid-Phase Microextraction (HS-SPME) and Simultaneous Distillation-Extraction (SDE) Coupled with GC-Olfactometry and GC-MS

Xu Yong-Quan,Wang Chao,Li Chang-Wen,Liu Shun-Hang,Zhang Chen-Xia,Li Li-Wei,Jiang Dong-Hua

Aroma volatiles from ripened and raw pu-erh tea were extracted by headspace solid-phase microextraction (HS-SPME) and simultaneous distillation-extraction (SDE). They were then characterized and identified using gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). The conditions of HS-SPME including fiber selections and sampling condition optimization have been previously investigated. With the two methods, 39 and 33 aroma-active compounds were detected and characterized in ripened and raw pu-erh tea samples, respectively. The aroma-active compounds with similar sensory descriptors were grouped into the same category, and the sum of individual aroma intensity values within each category showed that the floral aroma (33.01 %), stale/musty aroma (25.24 %), and woody aroma (11.17 %) were the major aroma categories in ripened pu-erh tea. Alcohols ( floral aroma notes), methoxyphenolic compounds ( stale/musty aroma notes), and ketones ( woody or floral aroma notes) play a vital role in the special flavor of ripened pu-erh tea. In raw pu-erh tea, the floral aroma (38.62 %) and fruity aroma (16.55 %) were the major aroma categories. These aromas were closely related to the characteristics of raw pu-erh tea aroma and its sensory perception.

研究领域: 食品科学 · 分析化学
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FOOD CHEMISTRY · 2023 · IF 8.8

Unraveling the contributing factors of stale odor in Longjing tea through a sensomics approach

Yanyan Cao,Chuangsheng Huang,Yating Guo,Yingxin Xu,Shuying Gong,Qiang Chu,Ping Chen

Longjing tea is renowned for its fresh aroma and high value. However, during storage, the emergence of an off-flavor known as “stale odor” can significantly impact the flavor quality and economic benefits of Longjing tea. Yet, the specific volatiles responsible for this stale odor in Longjing tea remain unknown. In this study, Longjing tea samples with varying degrees of stale odor intensity were analyzed using simultaneous distillation extraction coupled with gas chromatography-mass spectrometry (SDE-GC–MS). Through odor activity value (OAV) and fractional omission testing, hexanoic acid and trans -2-nonenal were identified as the primary contributors to the stale odor. Moreover, the concentration of hexanoic acid was found to be valuable in predicting the intensity of the stale odor in Longjing tea. The oxidative degradation of linoleic acid was proved as the generation pathway of stale odor in Longjing tea. These findings provide essential theoretical principles for Longjing tea production and preservation.

研究领域: 食品科学 · 农业化学 · 分析化学
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