CHROMATOGRAPHIA
·
2012
·Vol. 75
·期 23
·1421-1433
·
IF 1.195
Shu Jianjun,Li Chan,Liu Mingming,Liu Hanlan,Feng Xionghan,Tan Wenfeng,Liu Fan
Three alkoxyl-functionalized ionic liquids, 1-(3-triethoxysilyl propyl)-3-methyl imidazolium hexafluorophosphate (TESPMIM[PF 6 ]), 1-(3-triethoxysilyl propyl)-3-methyl imidazolium tetrafluoroborate (TESPMIM[BF 4 ]), and 1-(3-triethoxysilyl propyl)-3-methyl imidazolium bis(trifluoromethanesulfonyl)imide (TESPMIM[N(SO 2 CF 3 ) 2 ]), were synthesized and used as selective coating materials to prepare chemically bonded ionic-liquid-based organic–inorganic hybrid solid-phase microextraction (SPME) fibers by sol–gel technology. A possible mechanism of the sol–gel process is proposed, and the successful binding of ionic liquids to the formed silica substrate was confirmed by Fourier-transform infrared spectroscopy (FT-IR). These ionic-liquid-based sol–gel coatings have porous surface structure, high thermal stability, strong solvent resistance, wide pH application range, good coating preparation reproducibility, special selectivity, and extraction efficiency for both polar and nonpolar compounds, such as phenolic environmental estrogens, fatty acids, aromatic amines, alcohols, phthalate esters, and polycyclic aromatic hydrocarbons. The TESPMIM[PF 6 ]- and TESPMIM[BF 4 ]-coated fibers have much lower thermal stability (to 300 and 285 °C, respectively) than TESPMIM[N(SO 2 CF 3 ) 2 ]-coated fiber (to 454 °C). However, the selectivity of these two fibers is higher towards strong polar analytes, while lower towards medium polar or nonpolar analytes compared with TESPMIM[N(SO 2 CF 3 ) 2 ]-based fiber. This could be explained by the fact that different counteranions in ionic liquid structures have different steric hindrance, nucleophilicity, hydrophobicity, and ability to form hydrogen bonds, resulting in significant difference in the characteristics of the ionic-liquid-based SPME fibers, such as the surface morphology, thermal stability, selective extraction ability, etc. This work demonstrates that the performance of the ionic-liquid-based coatings can be simply tuned by changing the counteranions incorporated into the ionic liquid structures.
研究领域:
分析化学
·
材料科学
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DOI
高影响因子
Journal of Food Measurement and Characterization
·
2026
·
IF 3.6
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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高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2026
·
IF 10.6
Chenqing Zhang,Mengyao Qin,Zhuoyue Hou,Yanmei Shi,Yanhao Zhang,Weixia Zhu,Shusheng Zhang,Kai Hu
An electron-deficient 3D carborane-COF (CB-TAPM) was fabricated. • CB-TAPM was used as SPME fiber coating for extraction of PAHs. • High affinity of B-rich COF fiber due to unique structure and multiple interactions. • An ultrasensitive HS-SPME/GC–MS/MS method was developed for detection of PAHs. • Greenness of the developed approach was evaluated based on various metric tools. In this study, carborane covalent organic framework (CB-TAPM) with electron-deficient structure was synthesized and applied as coating material for solid-phase microextraction (SPME) fibers. The extraction efficiency of CB-TAPM COF-coated fibers for polycyclic aromatic hydrocarbons (PAHs) was systematically evaluated and demonstrated superiority over other investigated COF-coated fibers and commercial fibers. The superior enrichment capacity and selectivity of the fabricated fibers for PAHs were attributable to unique electron-deficient boron-rich mesoporous framework and high surface area, which can provide multiple interactions (e.g. hydrophobic effects, π-π stacking, B-H δ- ···H δ+ -C and size-matching effects) with the target analytes. Under the optimized conditions, the developed SPME/GC-MS/MS method demonstrated excellent linearity for target PAHs, with determination coefficients (R²) ranging from 0.9917 to 0.9999 across the calibration curves. The method achieved detection limits (LODs, S/N = 3) of 11–15 pg g −1 for PAHs in milk and 0.24–0.36 pg mL −1 in water samples, demonstrating exceptional sensitivity for complex matrices. Additionally, the fabricated fibers exhibited high repeatability (RSD < 8.6%, n = 5), and reproducibility (inter-batch RSD < 7.8%, n = 5) and reusability (>150 extraction-desorption cycles). This study demonstrates a sustainable and novel methodology for PAH extraction and analysis, while simultaneously broadening the scope of COF-based coatings for SPME applications. Download: Download high-res image (154KB) Download: Download full-size image
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高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2019
·
IF 3.714
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.
研究领域:
植物学
·
药理学
·
分析化学
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产品关联
DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2023
·
IF 6
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.
研究领域:
食品科学
·
分析化学
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产品关联
DOI
高影响因子
SENSORS AND ACTUATORS B-CHEMICAL
·
2023
·
IF 8.4
Nianlu Li,Mengping Zhang,Xiao Geng,Ranran Liu,Xiao Meng,Wei Zou,Wenwen Chen,Hua Shao,Cuijuan Wang
Poisoning with diquat (DQ) and paraquat (PQ) herbicides has been a public health problem. Unfortunately, rapid detection in biofluids remains challenging. Herein, a hyphenated approach of electro-enhanced adsorption, solid-phase microextraction, and surface-enhanced Raman spectroscopy (EE−SPME−SERS) was exploited for rapid and sensitive in situ analysis of DQ and PQ in human urine and plasma. A porous Ag fiber with an Au layer (p-Ag/Au fiber) was fabricated with multi-functions (SERS substrate, SPME sorbent , and working electrode). Clear trends could be observed between signal intensity and concentration of DQ or PQ with high reproducibility. The method detection limits (MDLs) calculated from the characteristic peak of DQ were 0.064 ppb and 0.65 ppb in urine and plasma, respectively. Corresponding MDLs for DQ and PQ in urine and plasma were 0.036 ppb and 0.35 ppb, respectively. The whole process of “extracting and detecting” was completed within 4 min with satisfactory recoveries. Notably, the EE−SPME−SERS technique could easily realize in situ analysis of DQ and PQ in biofluids with good selectivity, which is practical in clinical diagnosis. This EE−SPME−SERS method provides a potential avenue for efficient pretreatment and in situ poison detection in biological samples.
研究领域:
分析化学
·
毒理学
·
临床医学
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产品关联
DOI
高影响因子
Journal of Food Measurement and Characterization
·
2019
·Vol. 14
·期 1
·535-547
·
IF 1.415
Al-Dalali Sam,Zheng Fuping,Sun Baoguo,Chen Feng,Wang Peng,Wang Wenping
Zhengrong vinegar is one of the renowned popular condiments in China, which has been consumed around Hebei province for about 136 years. Its different processing steps are considered as important and critical steps that are responsible for the generation of representative flavors besides the acetic acid. An HS-SPME coupled with GC–MS method was used to evaluate the changes of the volatiles of the vinegar that were generated during the different processing steps including before adding salt (BAS), after adding salt (AAS), after filtration (AF) and final product (FP). In addition, aroma-active volatiles of the final vinegar product were characterized by GC-O coupled with detection frequency technique (modified frequency, MF%) that is a combination of aroma intensity and aroma frequency values that can be used to improve the description of a reliable data from GC-O. Among the 42 detected volatiles, 38 of them were positively identified by their corresponding authentic compounds. Besides, 24 volatiles were recognized as aroma-active volatiles. On the other hand, the content of individual volatile groups was decreased along with the continuation of the fermentation process from the BAS step to FP step, except the aldehydes group that displayed a slight increase. Of which, 2-pentylfuran and ethyl heptanoate disappeared in the AF and FP samples. The main contributors to the Zhengrong aroma profile that had MF (%) > 80 included isovaleric acid, 2-acetoxy-3-butanone, hexanoic acid, ethyl hexanoate, 3-(methylthio)propyl acetate, decanal and 2-phenyl-2-butenal, while the volatile compounds that had a middle MF in a range between 70 and 80 were 2-methylbutanoic acid, tetramethylpyrazine, nonanal, 1,2-dimethoxybenzene, 4-ethylphenol, ethyl benzoate, ethyl benzeneacetate, 2-phenylethyl acetate and 4-ethylguaiacol.
研究领域:
食品科学
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分析化学
·
风味化学
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DOI
高影响因子
FLAVOUR AND FRAGRANCE JOURNAL
·
2026
·
IF 2.5
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.
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高影响因子
FLAVOUR AND FRAGRANCE JOURNAL
·
2026
·
IF 2.5
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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DOI
高影响因子
Current Analytical Chemistry
·
2024
·Vol. 20
·期 9
·629-636
·
IF 1.7
Yangzhou Xie,Yi Yang,Yu Tian,Zhimin Liu,Zhigang Xu,Wei Jiang,Zhihua Liu,Xiaoxi Si
Background: Terpenoids are essential aroma substances in teas, and their concentration brings various characteristics to different teas. Therefore, developing a simple and stable method is necessary for distinguishing tea categories. Objective: In previous studies, more attention was paid to non-chiral isomers of terpenes due to the challenges of separating chiral isomers. So, this paper aims to present a method for effectively separating seven terpenoid substances, including chiral isomers and non-chiral isomers, to facilitate the classification and identification of teas. Methods: A method utilizing headspace solid-phase microextraction coupled with gas chromatography- mass spectrometry was used to isolate and analyze 7 terpenoid compounds. After optimized conditions, the BGB-176 chiral column and the PDMS/DVB fiber were selected for subsequent analysis. Results: This method has a good linear range of 0.1-200 mg/L, and its linear correlation coefficients are between 0.9974 and 0.9994, and the limit of detection and the limit of quantification is 0.02–0.03 and 0.06–0.09 mg/L, respectively. Only five terpenoid substances were detected in a total of 15 tea samples. Furthermore, In the detection of carvon and α-ionone optical isomers, the S isomer was mainly detected. Conclusions: An effective approach was developed to separate and analyze 7 terpenoid compounds in natural and synthetic teas. Meanwhile, 15 tea samples can be identified and classified using principal component analysis.
研究领域:
分析化学
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食品科学
·
植物化学
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DOI
高影响因子
FOOD CHEMISTRY
·
2021
·
IF 7.514
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.
研究领域:
食品科学
·
分析化学
·
茶叶加工技术
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产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2021
·
IF 4.952
Chen Liu,Ping Yang,Haili Wang,Huanlu Song
Yogurt is widely acknowledged as a healthy dairy product with unique aroma. However, the changes in the odor compounds often affect the storage and shelf life of yogurt. Besides, the complex colloidal system and low concentration levels of most of odorants make it more difficult to be analyzed. Therefore, this study extracted the odor compounds of yogurt through four extraction methods, including dynamic headspace sampling (DHS), solid phase micro-extraction (SPME), solvent-assisted flavor evaporation (SAFE), and Stir bar sorptive extraction (SBSE). A total of 117 odorants, including 27 esters, 27 alcohols, 22 ketones, 16 acids, 15 aldehydes, 5 sulfides, and 5 other compounds, were identified. Of which, 31 odor-active compounds were perceived, and 12 compounds were smelled for the first time in yogurt. Of the four methods, DHS showed the most outstanding extraction effect by obtaining 88 odor compounds. Around 13 volatiles were characterized as the key odor-active compounds of yogurt. Similarly, acetophenone and butyl acrylate were detected as the key odor-active compounds of yogurt for the first time. 2,3-Butanedione was the vital odor-active compound with the highest flavor dilution (FD) factor in yogurt. The results concluded that the odor-active compounds in yogurt might have synergistic and masking effects between them.
研究领域:
食品科学
·
分析化学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）