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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 RESEARCH INTERNATIONAL · 2024 · IF 7

Comprehensive determination of fatty acids in real samples without derivatization by DMU-SPME-GC methods

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

The comprehensive determination of fatty acids without derivatization, including short-chain fatty acids (SCFAs), medium-chain fatty acids (MCFAs) and long-chain fatty acids (LCFAs), is a big challenge but powerful for lipidomics in biology, food, and environment. Herein, the dual mode unity solid-phase microextraction (DMU-SPME) combined with gas chromatography-flame ionization detector (GC-FID) or mass spectrometry (MS) was proposed as a powerful method for the determination of comprehensive free fatty acids in real samples. Under the optimized DMU-SPME conditions, the proposed method has good linearity (R 2  ≥ 0.994) and low limits of determination (0.01–0.14 mg/L). In the stability analysis, the intra-day relative standard deviation was 1.39–12.43 %, and the inter-day relative standard deviation was 2.84–10.79 %. The recoveries of selected 10 fatty acids in real samples ranged from 90.18 % to 110.75 %, indicating that the method has good accuracy. Fatty acids ranging from C2 to C22 were detected in real samples by the untargeted determination method of DMU-SPME combined with gas chromatography-mass spectrometry (GC–MS). The DMU-SPME method proposed in this study can be used for lipid metabolism analysis and free fatty acid determination in the fields of biology, food, and environment.

CAS / MDL: 64-17-5
研究领域: 生物化学 · 食品科学 · 环境科学
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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 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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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2024 · IF 4

Characterization of key volatile flavor compounds in dried sausages by HS-SPME and SAFE, which combined with GC-MS, GC-O and OAV

Wang He,Zixuan Liu,Haoyue Liu,Jie Sun,Haitao Chen,Baoguo Sun

The flavor of three types dried sausage from Guangdong, Sichuan and Harbin were studied by headspace solid-phase microextraction (HS-SPME) and solvent-assisted flavor evaporation (SAFE) combined with gas chromatography-mass spectrometry (GC-MS), sensory evaluation combined with principal component analysis. The results showed that Harbin dried sausage had more prominent spicy flavor attributes, and the varieties and contents of flavor substances were more abundant. Then Harbin dried sausage was selected for further analysis. The flavor dilution factor of 37 aroma components was obtained by gas chromatography-olfactometry-mass spectrometry and aroma extract dilution analysis. 30 compounds were quantitated, and their odor activity values were calculated. The key aroma components were validated by using recombination and omission experiments. The omission experiment of 27 aroma compounds was carried out, and 10 compounds were finally determined as the key aroma active substance. The key aroma components of Harbin dried sausage included hexanoic acid, acetic acid, isovaleric acid, butyric acid , nonanal, acetoin, hydroxyacetone, ethyl hexanoate, eugenol, and p -cresol.

研究领域: 食品科学 · 分析化学
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CHROMATOGRAPHIA · 2014 ·Vol. 77 ·期 19 ·1379-1386 · IF 1.37

Characterization of Volatile Organic Metabolites in Lung Cancer Pleural Effusions by SPME–GC/MS Combined with an Untargeted Metabolomic Method

Liu Huijun,Li Caixia,Wang Hong,Huang Zhongping,Zhang Peipei,Pan Zaifa,Wang Lili

Headspace solid-phase microextraction and gas chromatography/mass spectrometry (HS-SPME–GC/MS) method combined with XCMS Online was tentatively applied to characterize the dysregulated volatile organic metabolites (VOMs) in benign and malignant pleural effusions. A total of 9 dysregulated feature groups were isolated from metabolic features in 35 pleural effusion samples (20 benign effusions and 15 malignant ones from lung cancer patients). Principle component analysis, partial least squares discriminant analysis (PLS-DA) and orthogonal PLS-DA were built to separate benign from malignant pleural effusion groups and to find dysregulated metabolites in significantly different amounts between the two groups. Four dysregulated VOMs such as 2-ethyl-1-hexanol, cyclohexanone, 1,2,4,5-tetramethylbenzene and naphthalene were selected according to the variable influence on the projection value. The concentration of the four dysregulated VOMs in benign and malignant effusions were further determined by external standard method. The median concentrations of 4 VOMs in malignant effusion samples were from 4.7 to 91,121.9 nM, whereas their median levels were only 1.9–318.3 nM in benign ones. The results show that the proposed SPME–GC/MS-based metabolomic approach combined with XCMS Online data processing is a simple, rapid and available method for the characterization of dysregulated VOMs in malignant and benign pleural effusions.

研究领域: 医学 · 分析化学 · 肿瘤学
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PACKAGING TECHNOLOGY AND SCIENCE · 2025 · IF 3.7

Development of an Aroma Permeation Measurement Method Using Dynamic SPME-GC-FID Technique Coupled to a Flow-Cell

Jian Zou,Gang Wang,Shuyu Duan,Chenyi Shi,Xiaobing Yun,Xiuhan Yang,Zhe Du,Huan Qiu,Winniford Bill

An isostatic aroma permeation measurement system was developed using a customized permeation cup and dynamic SPME-GC-FID coupled to a flow-cell unit. The limit of quantitation (LOQ) of the method ranged from 0.012 to 0.054 mg/m 3 with a PDMS-coated SPME Arrow, with typical linearity from 5 to 600 mg/m 3 . The system's repeatability on a polyethylene terephthalate (PET) film was between 8.7% and 25.0% (%RSD, n = 4). The results were verified using headspace GC–MS and thermal desorption GC–MS, with relative average deviation (%RAD) ranging from 6.0% to 20.7%. The aroma barrier performance of six film samples, including PET, biaxially oriented polypropylene (BOPP) and vacuum metalized polyethylene (PET//VMPE), was compared using this method with a mixture of five model aroma compounds, such as 2-methyl pyrazine, 2-heptanone and benzaldehyde. This method provides a sensitive, automated and low-cost solution for evaluating the aroma barrier performance of polymer films, with potential applications in the packaging industry.

CAS / MDL: 109-08-0
研究领域: 分析化学 · 食品科学与工程
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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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