SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang

Laoxianghuang, fermented from Citrus medica L. var. Sarcodactylis Swingle of the Rutaceae family, is a medicinal food. The volatiles of Laoxianghuang fermented in different years were obtained by solid-phase microextraction combined with gas chromatography–mass spectrometry (SPME-GC–MS). Meanwhile,...

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Main Authors: Liu Yaqun, Liu Hanxu, Lin Wanling, Xue Yingzhu, Liu Mouquan, Zheng Yuzhong, Hu Lei, Yang Yingkai, Chen Yidong
Format: Article
Language:English
Published: Frontiers Media S.A. 2022-08-01
Series:Frontiers in Nutrition
Subjects:
Online Access:https://www.frontiersin.org/articles/10.3389/fnut.2022.915776/full
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author Liu Yaqun
Liu Yaqun
Liu Hanxu
Lin Wanling
Lin Wanling
Xue Yingzhu
Liu Mouquan
Liu Mouquan
Zheng Yuzhong
Zheng Yuzhong
Hu Lei
Hu Lei
Yang Yingkai
Chen Yidong
author_facet Liu Yaqun
Liu Yaqun
Liu Hanxu
Lin Wanling
Lin Wanling
Xue Yingzhu
Liu Mouquan
Liu Mouquan
Zheng Yuzhong
Zheng Yuzhong
Hu Lei
Hu Lei
Yang Yingkai
Chen Yidong
author_sort Liu Yaqun
collection DOAJ
description Laoxianghuang, fermented from Citrus medica L. var. Sarcodactylis Swingle of the Rutaceae family, is a medicinal food. The volatiles of Laoxianghuang fermented in different years were obtained by solid-phase microextraction combined with gas chromatography–mass spectrometry (SPME-GC–MS). Meanwhile, the evolution of its component-flavor function during the fermentation process was explored in depth by combining chemometrics and performance analyses. To extract the volatile compounds from Laoxianghuang, the fiber coating, extraction time, and desorption temperature were optimized in terms of the number and area of peaks. A polydimethylsiloxane/divinylbenzene (PDMS/DVB) with a thickness of 65 μm fiber, extraction time of 30 min, and desorption temperature of 200 °C were shown to be the optimal conditions. There were 42, 44, 52, 53, 53, and 52 volatiles identified in the 3rd, 5th, 8th, 10th, 15th, and 20th years of fermentation of Laoxianghuang, respectively. The relative contents were 97.87%, 98.50%, 98.77%, 98.85%, 99.08%, and 98.36%, respectively. Terpenes (mainly limonene, γ-terpinene and cymene) displayed the highest relative content and were positively correlated with the year of fermentation, followed by alcohols (mainly α-terpineol, β-terpinenol, and γ-terpineol), ketones (mainly cyclohexanone, D(+)-carvone and β-ionone), aldehydes (2-furaldehyde, 5-methylfurfural, and 1-nonanal), phenols (thymol, chlorothymol, and eugenol), esters (bornyl formate, citronellyl acetate, and neryl acetate), and ethers (n-octyl ether and anethole). Principal component analysis (PCA) and hierarchical cluster analysis (HCA) showed a closer relationship between the composition of Laoxianghuang with similar fermentation years of the same gradient (3rd-5th, 8th-10th, and 15th-20th). Partial least squares discriminant analysis (PLS-DA) VIP scores and PCA-biplot showed that α-terpineol, γ-terpinene, cymene, and limonene were the differential candidate biomarkers. Flavor analysis revealed that Laoxianghuang exhibited wood odor from the 3rd to the 10th year of fermentation, while herb odor appeared in the 15th and the 20th year. This study analyzed the changing pattern of the flavor and function of Laoxianghuang through the evolution of the composition, which provided a theoretical basis for further research on subsequent fermentation.
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spelling doaj.art-77b524e20c1f40ec9996cb04f691bede2022-12-22T02:13:25ZengFrontiers Media S.A.Frontiers in Nutrition2296-861X2022-08-01910.3389/fnut.2022.915776915776SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of LaoxianghuangLiu Yaqun0Liu Yaqun1Liu Hanxu2Lin Wanling3Lin Wanling4Xue Yingzhu5Liu Mouquan6Liu Mouquan7Zheng Yuzhong8Zheng Yuzhong9Hu Lei10Hu Lei11Yang Yingkai12Chen Yidong13School of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaGuangdong Provincial Key Laboratory of Functional Substances in Medicinal Edible Resources and Healthcare Products, Chaozhou, ChinaSchool of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaSchool of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaGuangdong Provincial Key Laboratory of Functional Substances in Medicinal Edible Resources and Healthcare Products, Chaozhou, ChinaChaozhou Branch of Chemistry and Chemical Engineering Guangdong Laboratory (Hanjiang Laboratory), Chaozhou, ChinaSchool of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaGuangdong Provincial Key Laboratory of Functional Substances in Medicinal Edible Resources and Healthcare Products, Chaozhou, ChinaSchool of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaGuangdong Provincial Key Laboratory of Functional Substances in Medicinal Edible Resources and Healthcare Products, Chaozhou, ChinaSchool of Food Engineering and Biotechnology, Hanshan Normal University, Chaozhou, ChinaGuangdong Provincial Key Laboratory of Functional Substances in Medicinal Edible Resources and Healthcare Products, Chaozhou, ChinaGuangdong Jigong Healthy Food Co., Ltd, Chaozhou, ChinaGuangdong Jigong Healthy Food Co., Ltd, Chaozhou, ChinaLaoxianghuang, fermented from Citrus medica L. var. Sarcodactylis Swingle of the Rutaceae family, is a medicinal food. The volatiles of Laoxianghuang fermented in different years were obtained by solid-phase microextraction combined with gas chromatography–mass spectrometry (SPME-GC–MS). Meanwhile, the evolution of its component-flavor function during the fermentation process was explored in depth by combining chemometrics and performance analyses. To extract the volatile compounds from Laoxianghuang, the fiber coating, extraction time, and desorption temperature were optimized in terms of the number and area of peaks. A polydimethylsiloxane/divinylbenzene (PDMS/DVB) with a thickness of 65 μm fiber, extraction time of 30 min, and desorption temperature of 200 °C were shown to be the optimal conditions. There were 42, 44, 52, 53, 53, and 52 volatiles identified in the 3rd, 5th, 8th, 10th, 15th, and 20th years of fermentation of Laoxianghuang, respectively. The relative contents were 97.87%, 98.50%, 98.77%, 98.85%, 99.08%, and 98.36%, respectively. Terpenes (mainly limonene, γ-terpinene and cymene) displayed the highest relative content and were positively correlated with the year of fermentation, followed by alcohols (mainly α-terpineol, β-terpinenol, and γ-terpineol), ketones (mainly cyclohexanone, D(+)-carvone and β-ionone), aldehydes (2-furaldehyde, 5-methylfurfural, and 1-nonanal), phenols (thymol, chlorothymol, and eugenol), esters (bornyl formate, citronellyl acetate, and neryl acetate), and ethers (n-octyl ether and anethole). Principal component analysis (PCA) and hierarchical cluster analysis (HCA) showed a closer relationship between the composition of Laoxianghuang with similar fermentation years of the same gradient (3rd-5th, 8th-10th, and 15th-20th). Partial least squares discriminant analysis (PLS-DA) VIP scores and PCA-biplot showed that α-terpineol, γ-terpinene, cymene, and limonene were the differential candidate biomarkers. Flavor analysis revealed that Laoxianghuang exhibited wood odor from the 3rd to the 10th year of fermentation, while herb odor appeared in the 15th and the 20th year. This study analyzed the changing pattern of the flavor and function of Laoxianghuang through the evolution of the composition, which provided a theoretical basis for further research on subsequent fermentation.https://www.frontiersin.org/articles/10.3389/fnut.2022.915776/fullLaoxianghuangSPME-GC-MSfermentation timevolatile componentsflavorfunction
spellingShingle Liu Yaqun
Liu Yaqun
Liu Hanxu
Lin Wanling
Lin Wanling
Xue Yingzhu
Liu Mouquan
Liu Mouquan
Zheng Yuzhong
Zheng Yuzhong
Hu Lei
Hu Lei
Yang Yingkai
Chen Yidong
SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
Frontiers in Nutrition
Laoxianghuang
SPME-GC-MS
fermentation time
volatile components
flavor
function
title SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
title_full SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
title_fullStr SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
title_full_unstemmed SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
title_short SPME-GC–MS combined with chemometrics to assess the impact of fermentation time on the components, flavor, and function of Laoxianghuang
title_sort spme gc ms combined with chemometrics to assess the impact of fermentation time on the components flavor and function of laoxianghuang
topic Laoxianghuang
SPME-GC-MS
fermentation time
volatile components
flavor
function
url https://www.frontiersin.org/articles/10.3389/fnut.2022.915776/full
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