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Journal of Food Measurement and Characterization · 2026 · IF 3.6

Differentiation and characterization of volatile organic compounds from different parts of saffron based on HS-SPME-GC-MS

Zhao Xiaohan,Wang Liling,Yin Xianggang,Wu Linlin,Zheng Ying,Shao Qingsong,Zhou Yifeng,Huang Jun

Saffron ( Crocus sativus L. ) is a valuable perennial bulbous medicinal herb, often referred to as the “golden spice”. Although previous studies have investigated the non-volatile components and bioactive constituents in various parts of saffron, comprehensive profiles of its volatile organic compounds (VOCs) remained limited. This study employed headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) combined with cluster heatmaps, principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) to analyze and compare the VOCs in seven parts of Zhejiang-cultivated saffron, namely stigma (SS), petal (SP), pollen (SPO), filaments (SF), corms (SC), buds (SB), and leaves (SL). A total of 72 VOCs of saffron were identified, comprising 10 alcohols, 7 esters, 19 ketones, 7 aldehydes, 17 alkenes, and 12 other compounds. Among these, fatty acid methyl esters were the predominant VOC components in SC, whereas safranal or isophorone exhibited relatively higher abundances in the other six parts, which were also enriched in trimethylcyclohexane or cyclohexene derivatives. Cluster heatmaps and PCA grouped the seven saffron parts into three major clusters: SS, SPO and the remaining five parts. Furthermore, 15 significantly differential compounds were screened using the scatter loading plot (S-plot) of the OPLS-DA model combined with variable importance in the projection (VIP) values. Isophorone, 2,2,6-trimethylcyclohexane-1,4-dione (DOIP), and 2,6,6-trimethyl-1,3-cyclohexadiene-1-carbaldehyde (safranal) were identified as common key discriminant compounds across all comparisons, and while SS, SP, SF, SB and SL each contain unique marker compounds. These findings provide a scientific foundation for the authentication, quality assessment and comprehensive utilization of saffron resources.

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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Authentication of chaste honey adulterated with high fructose corn syrup by HS-SPME-GC-MS coupled with chemometrics

Quanzeng Wei,Juntao Sun,Jiaqi Guo,Xiaofei Li,Xiaohua Zhang,Fugang Xiao

The adulteration of the honey industry is serious, especially the syrup adulteration method is difficult to detect. To develop the detection technology of chaste honey adulteration with high fructose corn syrup (HFCS), the condition of headspace solid-phase micro-extraction (HS-SPME) was optimized for extracting the volatile compounds of chaste honey. HS-SPME conditions were selected for optimization using Plackett Burman, steepest ascent and Box-Behnken. Volatile compounds from chaste honey adulterated with HFCS were analyzed by gas chromatography-mass spectrometry (GC-MS). M/Z RT pairs data from differences in chaste honey contents in HFCS-adulterated samples were analyzed by linear discriminant analysis (LDA), principal component analysis (PCA), and artificial neural network (ANN). The results indicated distinguished adulterated chaste honey at different proportions was not ideal using LDA and PCA. A back propagation (BP) artificial neural network (ANN)model was constructed based on m/z RT pair data. Correlation coefficients of training, verification, testing and comprehensive data of BP-ANN were 0.994, 0.945, 0.968 and 0.979, respectively, indicating good accuracy of the BP-ANN prediction model. The present study discusses a new strategy that determined the chaste honey contents in HFCS-adulterated samples as well as did not rely on the identification of volatile compounds.

CAS / MDL: 93-89-0
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2019 · IF 3.714

Chemical composition and biological activities of essential oil isolated by HS-SPME and UAHD from fruits of bergamot

Chen Xing,Chunqing Qin,Xueqing Li,Fuming Zhang,Robert J. Linhardt,Peilong Sun,Anqiang Zhang

Bergamot essential oil (BEO), which is extracted from bergamot fruit peel, has many health benefits such as improving blood circulation and anticancer activity. In this paper, volatile components were obtained by headspace solid phase microextraction (HS-SPME) and ultrasound-assisted hydrodistillation (UAHD) from the fruits of bergamot ( Citrus medica L. var. sarcodactylis (Noot.) Swingle). The oil yield of BEO from UAHD extraction was 0.48%, which is 118% higher than that of hydrodistillation (HD). The chemical compositions of the volatile components were analyzed using GC-MS. A total of 46 volatile compounds belonging to distinct chemical families were identified. The major components were identified as d -limonene (60.44%), γ-terpinene (20.28%). The biological activities, including antimicrobial activities and antioxidant activities of BEO were detected. The BEO exhibited activities against bacteria and fungi with minimal inhibitory concentration (MIC) values in the range of 0.78–3.13 μL/mL and minimum bactericidal or fungicidal concentration (MBC/MFC) values in the range of 1.56–6.25 μL/mL. BEO showed strong activity against E. coli (MIC = 0.78 μL/mL, MBC = 1.56 μL/mL). BEO also showed substantial antioxidant activity based on ferric reducing antioxidant power (FRAP) assay for reducing power, 2,2′-azino-bis(3-ethyl benzothiazoline-6-sulfonic acid) (ABTS) assay for radical scavenging activity, and superoxide anion radical scavenging activity.

CAS / MDL: 1397-89-3 64-75-5
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MICROCHIMICA ACTA · 2024 ·Vol. 192 ·期 1 ·1-12 · IF 5.3

A colorimetric sensor for the sensitive and rapid detection of ampicillin based on CS-Cu,Fe/HS nanozyme

Hou Linqian,Wei Jinya,Xiang Chen,Yang Dezhi,Yang Yaling

A novel copper and iron doped containing chitosan and heparin sodium carbon dots (CS-Cu,Fe/HS) nanozyme was formulated through a single-step microwave digestion method. CS-Cu,Fe/HS exhibits excellent peroxidase (POD)-like activity and positive charge characteristics, and it can oxidize the negatively charged 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) in the presence of H 2 O 2 to produce a green compound (ox-ABTS). Furthermore, CS-Cu,Fe/HS enhances electron transfer and provides additional active sites through the valence state transformations of Fe 2+ /Fe 3+ and Cu 2+ /Cu + . Interestingly, the POD-like activity of CS-Cu,Fe/HS is inhibited with the introduction of ampicillin (AMP), which may be because the Cu and Fe ions in CS-Cu,Fe/HS form complexes with AMP, leading to changes in the structure or surface properties of the nanozyme, thereby reducing the number of active sites on the nanozyme. Drawing from this, a straightforward and reliable colorimetric sensor was constructed for AMP detection, featuring a linear range of 0.033 to 110 μg/mL and a detection limit as low as 11.6 ng/mL. The proposed detection method for AMP performed well in real samples, with recoveries ranging from 94.8% to 110.2%. Graphical abstract

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FLAVOUR AND FRAGRANCE JOURNAL · 2026 · IF 2.5

Geographical Differences in Catimor Coffee Aroma: Comprehensive Volatile Analysis and Key Odour Identification by HS-SPME-GC-TOF-MS

Hongyan Chen,Xian Chen,Na Wang,Xin Fan,Qi Zhang,Lunzhao Yi

Catimor coffee, an economically significant cultivar known for its disease resistance and high yield potential. By integrating headspace solid-phase microextraction gas chromatography time-of-flight mass spectrometry (HS-SPME-GC-TOF-MS) with relative odour activity value (ROAV) analysis, we systematically characterised the aroma compounds from four Yunnan and two Laotian production regions. A total of 183 dry aroma and 172 wet aroma compounds were identified, with ROAV analysis revealing significant geographical variations in both aroma profiles. Key odorants responsible for regional differentiation were identified and quantified. In dry aroma, ethyl isovalerate was established as the characteristic marker for fruity aroma in BS-1 samples, while LC-2 samples displayed a predominantly acidic profile. Wet aroma analysis showed PE-3 samples with strong floral, nutty and roasted characteristics, contrasted by Laos-6 samples exhibiting pronounced fruity, acidic and roasted notes. Critical odour-active compounds including furfuryl acetate (fruity), acetic acid (sour), along with 2-acetylpyrrole, difurfuryl ether and furfuryl alcohol (roasted) were quantitatively confirmed as major contributors to specific flavour attributes. The research establishes a comprehensive volatile compound database for Catimor coffee and elucidates the chemical foundation of regional aroma differences, providing scientific support for geographical origin authentication and quality enhancement in coffee production.

CAS / MDL: 64-17-5
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FLAVOUR AND FRAGRANCE JOURNAL · 2026 · IF 2.5

Characterisation of Volatile Profiles in Four Varieties of Jin'an Crispy Peaches Using HS-SPME-GC–MS and OAV Analysis

Wenjie Ye,Hongwei Lu,Han Chen,Naidong Chen,Li Zhang

Jin'an crispy peach is a famous geographical indication product widely grown in Lu'an City. In this study, four representative cultivars, including ‘Chunxue’, ‘Nanguohong’, ‘Chunmi’, and ‘Huangjinmi’, were selected to analyse their volatile compounds, and the headspace solid-phase microextraction (HS-SPME) method was employed. Fifty-eight volatile compounds were identified by gas chromatography–mass spectrometry (GC–MS), with 31, 24, 24, and 16 compounds detected in ‘Nanguohong’, ‘Chunxue’, ‘Chunmi’ and ‘Huangjinmi’, respectively. Principal component analysis (PCA) revealed strong correlations among five major compounds ( E )-2-hexenal, benzaldehyde, nonadienol, heptanoic acid and nonanoic acid in different cultivars. Odour activity value (OAV) analysis showed that 2-trans-4-trans-decadienal and β-damascenone exhibited the highest OAVs and together contributed to the primary flavour of the “Nanguohong” cultivar. In the “Chunxue” cultivar, ( E )-2-nonenal and 2,4-nonadien-1-al contributed to its grassy and green vegetable-like aromas. In the “Chunmi” and “Huangjinmi” cultivars, 2-ethyl-1-hexanol and phenylethyl alcohol were the predominant odour-active compounds and imparted a sweet aroma to the peaches. This research not only enhances our understanding of the flavour characteristics of Jin'an crispy peach but also lays a foundation for its further development and utilisation.

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JOURNAL OF CHEMICAL AND ENGINEERING DATA · 2022 · IF 3.119

Vapor–Liquid Equilibrium of α-Pinene, Longifolene, and Abietic Acid of Pine Oleoresin: HS-GC Measurements and Model Correlation

Shufen Wang,Xiaopeng Chen,Jiezhen Liang,Xiaojie Wei,Hairong Mo,Kaixi Deng,Linlin Wang

Investigating phase equilibrium on the terpenoid of the pine oleoresin system is of great importance for the usage relevant to the oleoresin. Herein, the binary and ternary isothermal vapor–liquid equilibrium (VLE) of α-pinene, longifolene, and abietic acid (three main components of oleoresin) at 313.15, 323.15, and 333.15 K were measured by headspace gas chromatography (HS-GC). There was no azeotropic behavior observed of α-pinene and longifolene. Abietic acid’s influence on separating α-pinene and longifolene was discussed. The relative volatilities of α-pinene and longifolene decrease in the presence of abietic acid, indicating a negative impact of abietic acid on their separation. The experimental data were correlated well with the nonrandom two-liquid, universal quasichemical, and Wilson models. The binary interaction parameters for each equation were also obtained, and the largest mean relative deviation of vapor-phase mole fraction and the largest absolute average deviation of pressure are 0.1975% and 0.0856 kPa, respectively.

CAS / MDL: 80-56-8 475-20-7
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FOOD CHEMISTRY · 2021 · IF 7.514

HS-SPME and GC/MS volatile component analysis of Yinghong No. 9 dark tea during the pile fermentation process

Wenji Zhang,Junxi Cao,Zhigang Li,Qiuhua Li,Xingfei Lai,Lingli Sun,Ruohong Chen,Shuai Wen,Shili Sun,Zhaoxiang Lai

Each type of tea has a unique volatile profile due to its variety, processing technologies and origin. Using HS-SPME and GC/MS, we analyzed the changes of volatile components in cultivar Yinghong No. 9 during pile-fermentation every 10 days. A total of 94 compounds showed significant differences during a total of 60 days mainly including alkanes, ketones, esters, terpenes, aromatics and heterocyclic compounds. Interestingly, 13 metabolites were progressively reduced during the first 20 days and remained unchanged in subsequent procedures, while 17 metabolites remained unchanged in the early stage and progressively increased during the last 20 days of pile fermentation, indicating that they are characteristic volatile compounds of raw material sun-dried green tea and dark tea, respectively. β-ionone, phenylethyl alcohol, and a-ionone could be the top three contributed aroma compounds in the final dark tea. Our study provides a theoretical basis for process and quality improvement of Yinghong No. 9.

CAS / MDL: 629-62-9
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JOURNAL OF SOLID STATE ELECTROCHEMISTRY · 2023 · IF 2.5

A simple electrochemical biosensor based on HS-β-cyclodextrin coordination methanobactin/gold nanoparticles for highly sensitive detection of nitrite

Chen Linlin,Song Jiaqi,Wang Ling,Hao Xi,Zhang Haipeng,Li Xintong,Wu Jiashu

Nitrite ( \(\mathrm{{NO}_2}^{-}\) ) is often added to food as a food additive, but the overuse of nitrite will pose a threat to human health, so it is important to establish a rapid detection method for nitrite in related food. In this work, gold nanoparticles (AuNPs) were synthesized by in situ reduction of methanobactin (Mb); it is a small bioactive peptide. HS-β-cyclodextrin (HS-β-CD) with supramolecular recognition function was coordinated with Mb/AuNPs by Au-S bond to form HS-β-CD@Mb/AuNPs. HS-β-CD@Mb/AuNPs were modified onto the surface of gold electrode by electrodeposition to successfully prepare the biosensor (HS-β-CD@Mb/AuNPs/Au). The HS-β-CD@Mb/AuNPs/Au was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), ultraviolet spectroscopy (UV), Fourier infrared spectroscopy (FTIR), fluorescence spectrometer (FL), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The established biosensor was successfully applied to the detection of nitrite in real samples, and the mechanism of NO 2 − oxidation was analyzed. The detection limit of the established detection system was as low as 0.013 μM in the linear range of 0.1–10,000 μM, the recoveries were 96.53–102.54%, and the selectivity of the sensor is demonstrated by anti-interference experiment. Also compared to the previously described electrochemical sensors, the newly developed ones have better sensitivity (50.7137 μA μM −1  cm −2 ) and selectivity. These results suggest that the work provides a new way for the accurate monitoring of nitrite in environmental and food safety.

CAS / MDL: 16961-25-4
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Distinguishing raw pu-erh tea production regions through a combination of HS-SPME-GC-MS and machine learning algorithms

Zhichao Xiong,Wanzhen Feng,Dongzhou Xia,Jixin Zhang,Yuming Wei,Tiehan Li,Junlan Huang,Yujie Wang,Jingming Ning

The authenticity of the geographical origin of agricultural products has received widespread attention. Tea tree varieties, processing processes and origins influence the quality and price of raw pu-erh tea (RPT). This study distinguished RPT from 10 different production areas through headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) combined with orthogonal partial least squares–discriminant analysis (OPLS-DA) model and machine learning algorithms. Among the thirty-five types of common volatiles identified, pentanal, heptanal, naphthalene, cedrol, and 2,6-di- tert -butylbenzoquinone were considered the key differential compounds distinguishing the 10 different production areas of the RPT samples through the screening of variable importance in projection values of the OPLS-DA and coefficient weights of the linear discriminant analysis function. Among them, heptanal and 2,6-di- tert -butylbenzoquinone had the highest content in West of Bingdao and the lowest content in Nannuoshan. The random forest algorithm achieved a discrimination accuracy of 98.4% based on the discrimination of five key compounds in 63 RPT samples. The random forest model was demonstrated to be reliable and valid by using receiver operating characteristic curves (area under the curve = 0.7603). The study results serve as a reference for the differentiation of 10 production areas of RPT.

CAS / MDL: 110-38-3
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ANALYTICAL CHEMISTRY · 2023 · IF 7.4

HS–SPME–GC–MS Untargeted Analysis of Normal Rat Organs Ex Vivo: Differential VOC Discrimination and Fingerprint VOC Identification

Yue Liu,Dianlong Ge,Jijuan Zhou,Yajing Chu,Xiangxue Zheng,Li Ke,Pan Li,Yan Lu,Xue Zou,Lei Xia,Yawei Liu,Chaoqun Huang,Chengyin Shen,Yannan Chu

The investigation of volatile organic compounds (VOCs) in human metabolites has been a topic of interest as it holds the potential for the development of non-invasive technologies to screen for organ lesions in vivo. However, it remains unclear whether VOCs differ among healthy organs. Consequently, a study was conducted to analyze VOCs in ex vivo organ tissues obtained from 16 Wistar rats, comprising 12 different organs. The VOCs released from each organ tissue were detected by the headspace-solid phase microextraction-gas chromatography-mass spectrometry technique. In the untargeted analysis of 147 chromatographic peaks, the differential volatiles of rat organs were explored based on the Mann–Whitney U test and fold change (FC > 2.0) compared with other organs. It was found that there were differential VOCs in seven organs. A discussion on the possible metabolic pathways and related biomarkers of organ differential VOCs was conducted. Based on the orthogonal partial least squares discriminant analysis and receiver operating characteristic curve, we found that differential VOCs in the liver, cecum, spleen, and kidney can be used as the unique identification of the corresponding organ. In this study, differential VOCs of organs in rats were systematically reported for the first time. Profiles of VOCs produced by healthy organs can serve as a reference or baseline that may indicate the presence of disease or abnormalities in the organ’s function. Differential VOCs can be used as the fingerprint of organs, and future integration with metabolic research may contribute to the development of healthcare.

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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
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