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HS-SPME-GC
FLAVOUR AND FRAGRANCE JOURNAL · 2023 ·Vol. 38 ·期 3 ·204-216 · IF 2.6

Analysis of volatile components in different broken rice by HS-SPME/GC-TOFMS

Kaixiong Peng,Qunyong Tang,Yuhan Zheng,Fang Ji,Xiaoming Chen

In this study, headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) was used to detect and analyse the volatile components of five samples with different degrees of fragmentation, combined with cluster analysis, orthogonal partial least squares discrimination analysis (OPLS-DA) and relative odour activity value (ROAV) analysis. The results showed that 70 volatile components were detected and identified in samples with different degrees of fragmentation. 40 were co-containing components. Cluster analysis revealed a high degree of similarity between samples B (20 mesh sieve top) and C (40 mesh sieve top), which were grouped into one category. The order of variation in the relative content of volatile components was A (unbroken) > E (120 mesh sieve top) > D (80 mesh sieve top) > B. C; the OPLS-DA analysis revealed significant differences in the volatile composition of rice samples with different degrees of fragmentation, This variation between samples is mainly due to the relative content of volatile components of 36 projections of variable importance (VIP > 1), such as ethyl butyrate, ethyl phenylacetate, and dimethyl trisulfide. A total of 12 volatile components with ROAV > 1, including ethyl hexanoate, 2-acetyl-1-pyrroline, and E -2-nonenal, were found to be the key volatile components in five samples based on their ROAV, the different degrees of crushing had a greater impact on the overall aroma of the rice, and the results can be used as a reference for further rice processors.

研究领域: 食品科学 · 分析化学
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FOOD CONTROL · 2022 · IF 6.652

Rapid and sensitive quantitation of DDMP (2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one) in baked red jujubes by HS-SPME-GC-MS/MS

Yening Qiao,Jinfeng Bi,Qinqin Chen,Xinye Wu,Xinwen Jin,Min Gou,Xinrui Yang,Giorgia Purcaro

Baked red jujube is a common food ingredient used to enrich the nutritional value and enhance the aroma. DDMP (2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one) with intense bitterness and potential toxicity may be present in several baked red jujube-based products but there are no well-defined methods to measure it quickly, sensitively, and accurately. Headspace solid-phase microextraction with gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS/MS) was applied for the analysis of DDMP. The standard curve was linear between the concentrations of 0.01 and 100 μg/mL, with a limit of detection at 0.1 ng/g that below the sensory threshold of DDMP (2.06 μg/g). Five cultivars of baked red jujubes from China were evaluated with the method for DDMP content (4.55–46.50 μg/g). The results indicated that jujube cultivars with a higher molar ratio of proline to glucose, lower moisture content, and stronger ability to resist water stress should be avoided from baking to modulate the formation of DDMP.

CAS / MDL: 110-54-3
研究领域: 食品科学 · 分析化学 · 植物学
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2020 ·Vol. 246 ·期 10 ·2065-2077 · IF 2.366

Determination of furan and its derivatives in preserved dried fruits and roasted nuts marketed in China using an optimized HS-SPME GC/MS method

Batool Zahra,Li Lin,Xu Dan,Wu Ming,Weng Longmei,Jiao Wenjuan,Cheng Hao,Roobab Umme,Zhang Xia,Li Xiaoxi,Liang Yi,Li Bing

Furan, which has been identified as possibly carcinogenic for humans, can be induced to different food items by thermal treatment. In accordance with the previous studies and risks associated with prevalence of furan in food, it is necessary to be acknowledged of amounts of furan formed in different thermally processed foods for human awareness. In this study, Headspace Solid-Phase Microextraction Gas Chromatography–Mass Spectrometry (HS-SPME-GC/MS) was optimized for simultaneous determination of furan, furfural, 2-methylfuran and 2-pentylfuran for the first time from different dried fruits and roasted nuts. The method was proved to be valid for determination of all analytes at 50 °C for 25 min, stirring at 700 rpm and 20% NaCl (W/V) using 50/30 μm divinlybenzene/carboxen/polysimethylsiloxane (DVB/CAR/PDMS) fibre. All analytes were baseline-separated at HP 5-MS column in less than 13 min and obtained results have shown prevalence of furan, furfural and 2-pentylfuran in the studied matrices; however, 2-pentylfuran was more prevalent in the roasted nuts than dried fruits and 2-methylfuran has not shown considerable prevalence in both matrices. Moreover, this method was validated in terms of linearity, precision, recovery, specificity, limit of detection and limit of quantification depending on analytes and sample matrices. Hence, the present method was proved to be highly sensitive, specific and robust with good precision and accuracy and suitable for monitoring these furan derivatives in the studied matrices.

研究领域: 食品安全 · 分析化学
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FOOD CHEMISTRY · 2025 · IF 9.8

Development of a fiber derivatization method for the analysis of 18 carbonyl compounds in roasted lamb using HS-SPME/GC-TQ/MS

Yingying Zhang,Yuan Wang,Huan Liu,Dasheng Xu,Dengyong Liu

A method based on headspace solid-phase microextraction fiber derivatization (HS-SPME-FD) coupled with gas chromatography-triple quadrupole mass spectrometry (GC-TQ/MS) was developed to quantify 18 flavor-related carbonyl compounds in roasted lamb. Optimization of derivatization conditions established the following optimal parameters: a 3 g/L concentration of O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), fiber loading at 50 °C for 5 min, followed by simultaneous extraction/derivatization at 50 °C for 30 min. The method was validated for linearity, limits of detection (LOD), limits of quantification (LOQ), precision, and accuracy. Results confirmed the method's suitability for determining carbonyl compounds in roasted lamb. During roasting, the composition and concentration of carbonyl compounds increased significantly, with hexanal being the most abundant. Additionally, the method detected carbonyl compounds in the model system at levels comparable to real roasted lamb, validating both the model's accuracy and the method's quantitative precision.

研究领域: 食品科学 · 分析化学
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Foods · 2025 ·Vol. 14 ·期 6 ·935 · IF 5.1

Comprehensive Characterization of Aroma Profile of “Glutinous Rice” Flavor in Pandanus amaryllifolius Roxb. Using HS–SPME–GC–O–MS and HS-GC-IMS Technology Coupled with OAV

Kun Tang,Cong Chen,Yutong Liu,Suxuan Li,Yiye Luo,Xiaoyu Chen,Zhiyong Wu

Pandan leaves have a prominent glutinous-rice aroma; however, few studies have explored their volatile aroma compound composition. Herein, the differences in the volatile aroma components of fresh and dried pandan leaves were investigated for the first time using HS–SPME–GC–O–MS combined with principal component analysis, orthogonal partial least squares discriminant analysis, and HS-GC-IMS with aroma fingerprinting. A total of 93 volatile compounds were identified, exceeding previous reports, including 43 main flavor components with odor activity values (OAV) > 1. OAV and aroma extract dilution analysis tests reveal 13 main aroma volatiles including 2-acetyl-1-pyrroline, hexanal, nonanal, phenylacetaldehyde, β-cyclocitral, butanal, ethyl caprylate, ethyl nonanoate, ethyl caprate, ethyl laurate, 3-hydroxy-2-butanone, acetophenone, and α-ionone. Sixteen types of aromas were classified, and the results are presented as flavor wheels. The findings of this study elucidate the changes and retention of aroma volatiles in differently processed leaves, which could benefit food industry applications.

研究领域: 食品科学 · 植物学
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FOOD CHEMISTRY · 2021 · IF 7.514

Discrimination and characterization of the volatile organic compounds in eight kinds of huajiao with geographical indication of China using electronic nose, HS-GC-IMS and HS-SPME-GC–MS

Xiya Feng,Hongwei Wang,Zhirong Wang,Pimiao Huang,Jianquan Kan

Huajiao ( Zanthoxylum bungeanum maxim. and Zanthoxylum armatum DC.) is a highly prized spice in China due to its distinctive aroma and taste. The volatile organic compounds (VOCs) of eight kinds of red and green huajiao which varied according to geographical indication of P.R. China were evaluated by electronic nose (E-nose), headspace solid-phase microextraction–gas chromatography-mass spectrometry (HS-SPME-GC–MS) and headspace-gas chromatography–ion mobility spectrometry (HS-GC-IMS). Results showed that red huajiao emitted more terpenes, esters, and fewer alcohols than green huajiao. Partial least squares-discriminant analysis based on GC–MS and GC-IMS data was revealed a good classifying tool for huajiao from different original habitats. Four and eight aroma substances were selected as the potential markers by the variable importance in projection (VIP) variable selection method, respectively. The results of the current study provide a useful basis in the huajiao aroma difference study. Additionally, a rapid huajiao aroma analysis method using GC-IMS was developed.

研究领域: 食品科学 · 植物化学
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MOLECULES · 2024 ·Vol. 29 ·期 3 ·567 · IF 4.2

Profiling of Volatile Compounds in ‘Muscat Hamburg’ Contaminated with Aspergillus carbonarius before OTA Biosynthesis Based on HS-SPME-GC-MS and DLLME-GC-MS

Yayun Guo,Zhe Wang,Yi He,Huanhuan Gao,Hongmei Shi

Aspergillus carbonariusis known to produce the carcinogenic ochratoxin A (OTA) in grapes. The metabolism process before OTA biosynthesis influences the content and composition of the volatile compounds in grapes. In this study, a self-established method based on QuEChERS coupled with high-performance liquid chromatography–fluorescence detection (HPLC-FLD) was used to determine the OTA levels during a seven-day contamination period. The results showed that OTA was detected on the second day after contamination withA. carbonarius. Thus, the first day was considered as the critical sampling timepoint for analyzing the volatiles in grapes before OTA biosynthesis. Additionally, the volatile compounds in grapes were analyzed using headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC-MS) and dispersive liquid–liquid microextraction gas chromatography–mass spectrometry (DLLME-GC-MS). The corresponding data were evaluated via multivariate data analysis using projection methods, including PCA and OPLS-DA. The results indicated significant differences in the nine volatile compounds in grapes contaminated withA. carbonariusbefore OTA biosynthesis. The results of the Pearson correlation analysis showed positive correlations between ethyl acetate, styrene, 1-hexanol and OTA; (E)-2-hexenal and nerolic acid were negatively correlated with OTA. Overall, these findings provide a theoretical basis for the early prediction of OTA formation in grape and grape products using GC-MS technology.Keywords:volatile compounds;Ochratoxin A;QuEChERS-HPLC-FLD;HS-SPME-GC-MS;DLLME-GC-MS;OPLS-DA

CAS / MDL: 7782-42-5
研究领域: 食品科学 · 真菌学 · 分析化学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Characterization of the volatile profile of feijoa (Acca sellowiana) fruit at different ripening stages by HS-SPME-GC/MS

Xinyue Song,Fen Dai,Jiarong Yao,Zhen Li,Zhongping Huang,Huijun Liu,Zuoyi Zhu

This study investigated the changes of volatile organic compounds (VOCs) in feijoa fruits during ripening. The VOCs were determined by head space solid phase microextraction and gas chromatography coupled to mass spectrometry (HS-SPME-GC/MS). Results showed that 78 VOCs were identified, mainly containing esters, terpenoids, aldehydes and alcohols. Only the minority of VOCs had relatively higher contents in unripe feijoa fruits, while most VOCs were highly accumulated in mid-ripe and ripe feijoa fruits. In the early stage, aldehydes and alcohols were the main flavor compounds which provided fruity and green aroma. The contribution of esters and terpenoids increased during the ripening process, leading to strong fruity and flower fragrance. Hexanal was the main volatile component of unripe feijoa fruits, while methyl benzoate, ethyl benzoate and 3-carene were the main volatile components of mid-ripe and ripe feijoa fruits. According to partial least square-discriminant analysis (PLS-DA), 17 VOCs with variable importance in the projection (VIP) > 1 could be used as significant markers to distinguish feijoa fruits during ripening. This study provided a theoretical support for the further study of the formation mechanism of VOCs in feijoa fruits during the ripening process.

CAS / MDL: 925-78-0
研究领域: 植物学 · 食品科学
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Foods · 2024 ·Vol. 13 ·期 24 ·3984 · IF 4.7

Exploring the Impact of Different Saccharomyces cerevisiae Strains on the Flavor Profile of Greengage Alcoholic Beverage Using GC-E-Nose, HS-GC-IMS, and HS-SPME-GC-MS

Zhenbao Shi,Wenzhe Li,Ziqiang Chen,Zhengcong Peng,Mingtao Ma,Jinglong Zhang,Dianhui Wu,Guangfa Xie,Jian Lu

Greengage alcoholic beverage (GAB) is gaining popularity for its distinctive fruity aroma and nutritional benefits. TheSaccharomyces cerevisiaestrain applied for fermentation significantly influences the metabolic production of aroma compounds, making the selection ofS. cerevisiaestrains to be critical for enhancing the unique flavor profile of the GAB in commercial production. In this study, the effects of two common commercialS. cerevisiaestrains (SY, EC-1118) and two laboratory-derived strains (ET008-c54, NM-8) on the flavor profile of the GAB were investigated. Volatile organic compounds (VOCs) of the GAB samples were analyzed using GC-E-Nose, HS-SPME-GC-MS, and HS-GC-IMS. Results showed significant differences in the flavor compound content of the GAB fermented by different strains. Nine VOCs were identified as potential markers by partial least squares–discriminant analysis (PLS-DA) combined with variable importance in projection (VIP), with ethyl esters playing a key role in distinguishing the aroma characteristics of different groups. Consequently, 13 aromatic compounds were selected and considered to be the typical VOCs of the GAB. Notably, β-ionone and ethyl octanoate emerged as representative aroma compounds, both showing the highest concentrations in the SY sample. These findings will provide valuable insights into the aroma differences of the GAB fermented by different strains and offer theoretical guidance for selecting suitable strains in the industrial production of the GAB.

研究领域: 食品科学 · 微生物学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2024 · IF 6

Characterization of the volatile flavour compounds in Yunnan Arabica coffee prepared by different primary processing methods using HS-SPME/GC-MS and HS-GC-IMS

Huinan Zhai,Wenjiang Dong,Yumei Tang,Rongsuo Hu,Xinxin Yu,Xiaoai Chen

In this study, coffee samples from seven primary processing methods—traditional dry processing (CG), dry processing I (GA), dry processing II (GB), traditional wet processing (CS), honey processing I (MA), honey processing II (MB), and honey processing III (MC)—underwent comprehensive investigation using HS-SPME/GC-MS and HS-GC-IMS. A total of 81 and 96 VOCs were identified by GC-MS and GC-IMS, respectively. The differences in VOCs among various primary processing samples were observed. The results demonstrated increased volatilization of coffee flavor substances due to anaerobic fermentation. CG, GA, and GB samples exhibited high levels of fruity, floral, and sweet aromas. Conversely, honey processing methods (MA, MB, and MC) enhanced the caramel, roasted aroma, and buttery flavor of coffee samples. PCA and PLS-DA successfully categorized coffee beans based on their aroma properties. These findings indicated that honey processing, combined with drying, significantly influenced coffee bean VOCs, enhancing caramel, roasted aroma, and buttery flavor—crucial for the characteristic volatile metabolites of Yunnan arabica coffee beans.

CAS / MDL: 106-35-4 67-56-1
研究领域: 食品科学 · 分析化学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2022 · IF 6.056

Identification of changes in the volatile compounds of robusta coffee beans during drying based on HS-SPME/GC-MS and E-nose analyses with the aid of chemometrics

Ke Zhang,Jinhuan Cheng,Qidi Hong,Wenjiang Dong,Xiaoai Chen,Guiping Wu,Zhenzhen Zhang

In this study, headspace solid-phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) and electronic-nose (E-nose) analyses were performed to examine the comprehensive flavor profiles of robusta coffee during heat air drying. A total of 62 volatile compounds were identified by HS-SPME/GC-MS, the level of acids, aldehydes, alcohols and esters decreased during drying process, however, the relative content of hydrocarbons and acids increased. Principal component analysis of the E-nose results clearly differentiated the samples related to drying time, and it was found that samples of initial stages (0 h, 3 h, and 6 h) had strong positive with different sensors. Partial least squares-discriminant analysis (PLS-DA) indicated that alcohols, ketones, and esters were the main contributing compounds to the flavour of coffee beans. The VIP score of PLS-DA larger than one illustrated that T30/1, T70/2, PA/2, and P30/2 were positive with ketones, sulfur compounds, and esters. These results could provide theoretical evidence about the change rule in volatile compounds of coffee beans during drying process, and could be applied to other thermally sensitive tropical agricultural products.

CAS / MDL: 106-35-4
研究领域: 食品科学 · 化学计量学
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FOOD CHEMISTRY · 2024 · IF 8.5

Identification and selection of volatile compounds derived from lipid oxidation as indicators for quality deterioration of frozen white meat and red meat using HS-SPME-GC–MS combined with OPLS-DA

Ligang Yu,Ying Pang,Guang Shen,Baoqing Bai,Yukun Yang,Maomao Zeng

This work aimed to investigate the effects of frozen storage on volatile compounds of white meats (chicken and duck) and red meats (pork, beef, and mutton). The samples were stored at −18 °C for 0, 2, 4, 10, 18 weeks, and volatile compounds were analyzed by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry. Results indicated that the total amounts of volatile compounds increased with frozen storage duration of meats. The correlations were observed between frozen storage duration and levels of 2-ethyl-1-hexanol, tetradecane, nonanal, decanal, octanal, tridecanal, benzaldehyde, pentadecane, propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester, heptadecane, and hexanal ( r  = 0.7456–0.9873). Levels of octanal and propanoic acid,2-methyl-,3-hydroxy-2,2,4-trimethylpentyl ester in white meat and benzaldehyde in red meat versus frozen storage duration fitted very well with zero-order reactions. Therefore, it was concluded that changes in volatile compounds derived from lipid oxidation may be used as indicators of quality deterioration during frozen storage of meat.

CAS / MDL: 13019-20-0
研究领域: 食品科学 · 分析化学
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