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INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY · 2024 ·Vol. 59 ·期 4 ·2689-2696 · IF 2.6

Bubble-driven solid-phase microextraction for the rapid determination of potassium sorbate in oyster sauce by HPLC-DAD

Jin-Yu Li,Yun-Jiao Ma,Feng Xiao,Xian-Bing Xu

Summary On-site sample preparation has the advantage of combining sampling and sample preparation into a single step, thereby minimising sources of error, and eliminating the risk of analyte instability. Bubble-driven solid-phase microextraction (BD-SPME) was first proposed as an on-site pretreatment method. Oyster sauce underwent on-site pretreatment to measure potassium sorbate levels via high-performance liquid chromatography with a diode array detector (HPLC-DAD), obviating the need for stirrers. The high sensitivity of the HPLC determination of potassium sorbate was obtained using BD-SPME pretreatment with a limit of detection (LOD) of 0.03 mg L −1 and a limit of quantification (LOQ) of 0.10 mg L −1 . The refined technique displayed remarkable linearity from 0.10 to 30.00 mg L −1 , boasting a coefficient of determination R 2 ≥ 0.998. In addition, the recoveries of potassium sorbate in oyster sauce using the method were in the range of 90.8–101.4%. Evidently, BD-SPME in combination with HPLC-DAD is a sensitive and promising analysis for on-site pretreatment.

研究领域: 分析化学 · 食品科学 · 化学工程
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Foods · 2020 ·Vol. 9 ·期 4 ·505 · IF 4.092

Volatile Organic Compounds Profiles to Determine Authenticity of Sweet Orange Juice Using Head Space Gas Chromatography Coupled with Multivariate Analysis

Qi Zhou,Guijie Li,Zhu Ou-Yang,Xin Yi,Linhua Huang,Hua Wang

An efficient and practical method for identifying mandarin juice over-blended into not from concentrate (NFC) orange juice was established. Juices were extracted from different cultivars of sweet orange and mandarin fruits. After being pasteurized, the volatile organic compounds (VOCs) in the juice samples were extracted using headspace solid-phase microextraction, and qualitatively and quantitatively analyzed using gas chromatography–mass spectrometry detection. Thirty-two VOCs contained in both the sweet orange juice and mandarin juice were used as variables, and the identification model for discriminating between the two varieties of juice was established by principal component analysis. Validation was applied by using common mandarin juices from Ponkan, Satsuma and Nanfengmiju cultivars blended at series of proportions into orange juices from Long-leaf, Olinda, and Hamlin cultivars. The model can visually identify a blending of mandarin juice at the volume fraction of 10% or above.Keywords:mandarin juice;not from concentrate (NFC);principal component analysis (PCA);headspace solid-phase microextraction (HS-SPME)

CAS / MDL: 108-94-1
研究领域: 食品科学 · 分析化学 · 农业化学
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FOOD CHEMISTRY · 2024 · IF 8.5

Evaluation of the effect of Torulaspora delbrueckii on important volatile compounds in navel orange original brandy using E–nose combined with HS–SPME–GC–MS

Jingjing Liu,Yin Wan,Yanru Chen,Haowei Fan,Mengxiang Li,Qihai Jiang,Guiming Fu

Simultaneous inoculation of non- Saccharomyces cerevisiae during the alcoholic fermentation process has been found to be an effective strategy for enhancing wine flavor. This study aimed to investigate the effect of Torulaspora delbrueckii NCUF305.2 on the flavor of navel orange original brandy (NOOB) using E–nose combined with HS–SPME–GC–MS. The results showed a significant increase ( p  < 0.05) in the sensitivity of NOOB to W5C, W3C, W1S, and W3S sensors by mixed fermentation (MF). Esters in NOOB increased by 4.13%, while higher alcohols increased by 21.93% ( p  < 0.001), terpenes and others increased by 52.07% and 40.99% ( p  < 0.01), respectively. Notably, several important volatile compounds with relative odor activity values above 10 showed an increase. Sensory analysis revealed that a more pronounced citrus-like flavor and higher overall appearance scores were found in MF than in pure fermentation (PF). These findings offer valuable theoretical guidance for enhancing the quality of fruit brandies.

CAS / MDL: 108-11-2
研究领域: 食品科学 · 微生物学
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MICROCHEMICAL JOURNAL · 2026 · IF 5.2

An in-tube SPME–based analytical strategy for simultaneous determination of multi-residue pesticides in environmental water samples using a MWCNTs-COOH/Polypyrrole nanocomposite coating

Kemiao Nan,Ran Jia,Weibo Feng,Shize Qu,Qi Shen,Yan Lin,Bing Zheng,Xiaodong Ma

Currently, the application of SPME techniques for multi-residue pesticide analysis is highly limited. In this study, a polypyrrole (PPy) doped with carboxylated multi-walled carbon nanotubes (MWCNTs-COOH) in-tube solid-phase microextraction (IT-SPME) nanocomposite was designed and fabricated by the electrodeposition method. The preparation parameters, such as Py concentration and MWCNTs-COOH content, were optimized. The morphology and structure of the coating were evaluated using SEM and FT-IR which revealed a distributed coating with a coarse and fine grid-like structure, achieving the desired structural integration. Additionally, experimental factors affecting extraction efficiency were optimized, such as sample volume, eluent type, etc. This method indicated a great linear range of 1–500 μg L −1 and high correlation coefficients (R 2 ) above 0.9971. The limit of detection (S/N = 3) and quantification (S/ N  = 10) were 0.12–1.27 μg L −1 and 0.41–4.22 μg L −1 . The relative standard deviations (RSDs) for intra-day and inter-day analyses were in the ranges of 1.02–12.17% and 3.10–13.15%, respectively. The method achieved satisfactory spiked recovery rates ranging from 80.34% to 103.23%. Furthermore, MWCNTs-COOH/PPy coating holds outstanding stability and selectivity. Therefore, the developed IT-SPME approach was successfully used in the analysis of actual environmental water samples.

CAS / MDL: 109-97-7
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Foods · 2025 ·Vol. 14 ·期 22 ·3946 · IF 5.1

Comparative Analysis of Volatile Organic Compounds in Freshwater-Cultured and Saline–Alkaline Selectively Bred Tilapia Using Electronic Nose, GC-IMS, and HS-SPME-GC-MS

Zhi Wang,Yi Yang,Dongxue Zhang,Jiashu Li,Longsheng Zhang,Yan Zhao,Jinliang Zhao,Junling Zhang,Jikui Wu

Tilapia is a cornerstone species in global aquaculture, yet the impact of saline-alkaline adaptive breeding on its flavor-related volatile organic compounds (VOCs) remains unclear. Herein, we compared VOCs in freshwater-cultured tilapia (FW) and 7th-generation tilapia subjected to long-term selective breeding for saline-alkaline tolerance (SAWG7) using an electronic nose (E-nose), gas chromatography-ion mobility spectrometry (GC-IMS), and headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). The aim was to identify flavor differentiation and assess the effect of saline-alkaline acclimation. E-nose analysis revealed distinct odor profiles, with SAWG7showing higher sensor responses for aldehydes, ketones, and alcohols. GC-IMS detected 32 VOCs, highlighting significant increases in alcohols, aldehydes, and heterocyclics in SAWG7. GC-MS identified 43 VOCs, with orthogonal partial least-squares discriminant analysis (OPLS-DA) confirming 18 discriminant compounds, including elevated ketones (2-undecanone), aldehydes ((E)-2-octenal), alcohols (2,7-Octadien-1-ol), and furans (2-ethyl-Furan) in SAWG7, linked to lipid oxidation under saline-alkaline stress. These findings demonstrate that long-term saline-alkaline breeding achieves a potentially more diverse VOC profile in tilapia by altering its volatile profiles. The study provides insights for optimizing aquaculture practices to improve product quality in marginal environments.

研究领域: 水产养殖 · 食品化学 · 分析化学 · 风味科学 · 环境胁迫生理学
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ACS Food Science & Technology · 2025 · IF 2.8

Investigation on the Flavor Characterization of Edible Cooked Insect Clanis Bilineata Larva Products Using SPME-GC-TOF/MS, UHPLC-MS/MS Combined with Sensory Evaluation

Zhimei Fan,Danni Zhang,Xueqian Guo,Yiwen Zhu,Panpan Chen,Chenxi Qiu,Ninglong Zhang,Jian Zhang,Liqiong Niu,Xichang Wang,Yuan Liu

Clanis Bilineata larva (CBL) is a unique Chinese insect delicacy in Jiangsu Province, which is known for its umami taste and high protein nutrition. To develop its desired flavor, the quantitative descriptive analysis (QDA) combined with high throughput instruments were applied to analyze the sensory attributes and compounds of raw, boiled and roasted CBLs. Through QDA, cooked CBLs showed higher meaty odor intensities than Raw CBL significantly (p < 0.05). Compared with boiled CBL, the roasting process could generate the roasted meaty/beany odors and umami/savory taste while reducing the negative effects of grassy/boiled vegetable/earthy odors and bitter taste. Pearson correlation analyses results showed that meaty odor was highly correlated with compounds produced by fatty acid degradation such as hexanal and 1-octen-3-ol. Meanwhile, histidine was highly correlated with bitter and adenosine monophosphate was highly correlated with umami. The taste and odor of cooked CBLs are mainly formed from the lipid degradation, protein degradation and nucleotide degradation. This study provides insights to use a proper cooking process to develop consumer-friendly CBL products.

CAS / MDL: 67-56-1 75-05-8
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MOLECULES · 2022 ·Vol. 27 ·期 14 ·4393 · IF 4.927

Discrimination and Characterization of the Volatile Organic Compounds in Schizonepetae Spica from Six Regions of China Using HS-GC-IMS and HS-SPME-GC-MS

Chao Li,Huiying Wan,Xinlong Wu,Jiaxin Yin,Limin Zhu,Hanjiang Chen,Xinbo Song,Lifeng Han,Wenzhi Yang,Heshui Yu,Zheng Li

Volatile organic compounds (VOCs) are the main chemical components ofSchizonepetae Spica(SS), which have positive effects on the quality evaluation of SS. In this study, HS-SPME-GC-MS (headspace solid-phase microextraction-gas chromatography-mass spectrometry) and HS-GC-IMS (headspace-gas chromatography-ion mobility spectrometry) were performed to characterize the VOCs of SS from six different regions. A total of 82 VOCs were identified. In addition, this work compared the suitability of two instruments to distinguish SS from different habitats. The regional classification using orthogonal partial least squares discriminant analysis (OPLS-DA) shows that the HS-GC-IMS method can classify samples better than the HS-SPME-GC-MS. This study provided a reference method for identification of the SS from different origins.Keywords:volatile organic compounds;Schizonepetae Spica;HS-SPME-GC-MS;HS-GC-IMS;OPLS-DA

CAS / MDL: 5989-54-8 591-24-2
研究领域: 药学化学 · 分析化学 · 中药学
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MOLECULES · 2024 ·Vol. 29 ·期 5 ·1142 · IF 4.2

Comparison of Flavonoid Content, Antioxidant Potential, Acetylcholinesterase Inhibition Activity and Volatile Components Based on HS-SPME-GC-MS of Different Parts from Matteuccia struthiopteris (L.) Todaro

Xin Wang,Jiatao Guo,Siqi Zang,Baodong Liu,Yuhuan Wu

Matteuccia struthiopterisis one of the most globally consumed edible ferns and widely used in folk medicine. Reports mainly focus on young fronds and the rhizome which are common edible medicinal parts. However, there are few detailed reports on other parts. Therefore, the volatile components of different parts based on HS-SPME-GC-MS were identified, and total flavonoid contents, antioxidant activities and acetylcholinesterase inhibitory activities were compared in order to reveal the difference of volatile components and potential medicinal value of different parts. The results showed that total flavonoid contents, antioxidant activities and volatile components of different parts were obviously different. The crozier exhibited the strongest antioxidant activities, but only underground parts exhibited a dose-dependent inhibition potential against AChE. Common volatile compounds were furfural and 2-furancarboxaldehyde, 5-methyl-. In addition, it was found that some volatile components from adventitious root, trophophyll, sporophyll and petiole were important ingredients in food, cosmetics, industrial manufacturing and pharmaceutical applications.

研究领域: 药理学 · 植物学 · 分析化学 · 药用植物
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FOOD RESEARCH INTERNATIONAL · 2025 · IF 8

Molecular sensory basis of the unique “cocoa aroma” in white tea: An integrated study combining HS-SPME-GC–MS, GC-O, molecular docking, and addition tests

Zhiqiang Zheng,Weiwei Wu,Zhihui Wang,Peng Zhang,Bangxing Ma,Yan Huang,Weijiang Sun

Cocoa aroma is a pleasant and highly market-accepted aroma type in white tea, yet its underlying key aroma components remain unclear. In this study, sensory quantitative descriptive analysis (QDA), gas chromatography–mass spectrometry (GC–MS), gas chromatography-olfactometry (GC-O), molecular docking , and aroma addition tests were employed to elucidate the aroma characteristics and aroma profile of cocoa aroma white tea (CCWT), traditional white tea (WT) and cocoa beans (CC), and then construct a comprehensive aroma flavor wheel. It was observed that CCWT consists of a composite aroma dominated by Cocoa aroma, accompanied by flowery, sweet, and herbal aroma. Ten compounds were identified as key aroma constituents in CCWT, including linalool , nerol , and β-ionone. Notably, isovaleraldehyde , 2-methylbutyraldehyde, and phenylacetaldehyde were identified as the primary aroma components contributing to the cocoa aroma. Molecular docking results revealed that 3 key aroma components generate cocoa aroma through hydrogen bonding and hydrophobic interactions with olfactory receptors , with binding energies of less than −4 kcal/mol. The addition tests indicated that isovaleraldehyde and 2-methylbutyraldehyde primarily contribute to the cocoa aroma in CCWT, while phenylacetaldehyde likely enhances this aroma through synergistic effects with other compounds. This research provides essential scientific support for enhancing white tea quality and guiding product development. A solid foundation has been established to facilitate sustainable growth of the broader tea industry.

研究领域: 食品科学 · 感官科学 · 分析化学 · 分子生物学 · 茶叶化学 · 香气化学
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JOURNAL OF CHROMATOGRAPHY A · 2026 · IF 4

Fabrication of a Robust Phenothiazine Hyper-crosslinked Polymer Coated Fiber for the Determination of Short-Chain Fatty Acids in Rat Faeces by HS-SPME/GC-FID

Chenqing Zhang,Juan Zhang,Zhiyu Zhang,Jing Yan,Zhuoyue Hou,Shusheng Zhang,Kai Hu

Short-chain fatty acids (SCFAs) are key biomarkers of gut microbiota activity and are implicated in various metabolic, inflammatory, and neurological diseases. This study fabricated a phenothiazine-based hyper-crosslinked polymer (PTZ-HCP) and applied it as a solid-phase microextraction (SPME) fiber coating for the analysis of nine SCFAs in rat feces by gas chromatography with flame ionization detection (GC-FID). The prepared PTZ-HCP was characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, N 2 adsorption-desorption measurements, and thermogravimetric analysis. These analyses confirmed its successful synthesis and revealed a porous structure, high specific surface area, and excellent thermal stability. Owing to these structural advantages and the capability for multiple functional groups, the PTZ-HCP coatings demonstrated outstanding extraction efficiency and high adsorption capacity for SCFAs. An SPME/GC-FID method using PTZ-HCP coated fibers were established and validated. The validation results demonstrated significant advantages, including a wide linear range (1.0 × 10 -3 -0.50 μg·mL -1 for 2-methylvaleric acid; 1.0 × 10 -3 -2.0 μg·mL -1 for 4-methylvaleric acid), low LODs (3.0 × 10 -4 μg·mL -1 for 2-methylvaleric acid and 4-methylvaleric acid), and good precision (≤ 9.5%). This work presents a novel SPME coating material that effectively addresses key challenges in the extraction and analysis of SCFAs in rat fecal samples. Moreover, it verifies that Coptis chinensis modulates gut microbiota by altering SCFA levels, thereby offering important insights for research on the pathological mechanisms and treatment of Parkinson’s disease.

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FOOD RESEARCH INTERNATIONAL · 2023 · IF 8.1

Comparison and discrimination of the terpenoids in 48 species of huajiao according to variety and geographical origin by E-nose coupled with HS-SPME-GC-MS

Yuanyuan Shao,Xiaoqiong Liu,Zhuoya Zhang,Pengxiang Wang,Kaikai Li,Chunmei Li

The unique flavor and aroma characteristics of huajiao were not only influenced by cultivated varieties, maturity, but also geographic origin. This study compared the terpenoids of 48 species of huajiao using headspace solid-phase microextraction–gas chromatography-mass spectrometry (HS-SPME-GC–MS) and electronic nose (E-nose). The E-nose results showed differences in huajiao from different origins and varieties, and from the PCA loading plots it was possible to conclude that some samples contained higher levels of hydrocarbons and alcohols, providing a preliminary discrimination between different species of huajiao. Further, GC-MS results showed that six key biomarkers could be used to distinguish red and green huajiao. Red huajiao in Central China contained more terpenoids than in other regions. Nine key biomarkers could be used to distinguish red huajiao from different regions. Oil huajiao exhibited a more distinct aroma in red huajiao. Green huajiao from Yunnan Province had more terpenoids than that from other provinces. The terpenoids content of Yunnan zhuyeqing was higher than other green huajiao. Heatmap analysis helped to find the most contributors of huajiao, which could be used as key terpenoids to differentiate huajiao of different regions or cultivars. Finally, through the correlation analysis of E-nose and GC-MS, it was found that the E-nose sensors could distinguish different huajiao by specific responses to some terpenoids in the samples.

CAS / MDL: 124-18-5
研究领域: 植物学 · 食品科学 · 分析化学
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FOOD CHEMISTRY · 2023 · IF 8.8

Characterization of the key odor-active compounds in different aroma types of Fu brick tea using HS-SPME/GC-MSO combined with sensory-directed flavor analysis

Xuexue Zheng,Tengfei Hu,He Xie,Xingchang Ou,Jianan Huang,Chao Wang,Zhonghua Liu,Qin Li

Fu brick tea (FBT) is popular for its unique ‘fungal flower’ aroma, however, its key odor-active compounds are essentially unknown. In this study, the odor-active compounds of “stale-fungal” aroma (CJX), “fresh-fungal” aroma (QJX), and “fermentation-fungal” aroma (FJX) types FBT were extracted and examined by headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC–MS) and gas chromatographyolfactometry (GC-O). A total of 43 volatile and 38 odor-active compounds were identified by these methods. Among them, the content of dihydroactindiolide (4596–13189 µg/L), (E) -linalool oxide (2863–6627 µg/L), and benzyl alcohol (4992–6859 µg/L) were highest. Aroma recombination experiments further verified that these odor-active compounds could be simulated the overall aroma profile of FBT successfully. Furthermore, omission experiments confirmed that 15, 20, and 15 key odor-active compounds in CJX, QJX, and FJX FBT, respectively. This study will provide a theoretical basis for comprehensively understanding the formation of characteristic aromas in FBT.

研究领域: 食品科学 · 分析化学
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