Analytical Methods
·
2023
·Vol. 15
·期 6
·849-858
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IF 3.1
Dandan Li,Xinxing Jiang,Yaxue Zhang,Wenxia Xue,Jihong Fu
A novel approach based on polydimethylsiloxane/graphene oxide/deep eutectic solvent (PDMS/GO/DES) sponge headspace solid phase extraction followed by GC-MS was successfully developed to determine the volatile components in cumin. The PDMS/GO/DES exhibits outstanding properties with high adsorption capacity and good chemical stability, and has shown its potentiality as an ideal adsorbent for the extraction of volatile compounds. The influence factors of the extraction process were investigated. Excellent analytical performances were achieved, including wide linearity (0.60–107.72 ng) with high correlation coefficients (R2 ≥ 0.9951), low LODs (0.23–9.23 ng) and LOQs (0.54–18.47 ng), satisfactory precision (intra-day RSDs ≤ 2.85% and inter-day RSDs ≤ 3.92%). Under the optimal extraction conditions, the volatile components in 17 cumin samples from four origins in Xinjiang were analyzed and 31 compounds were identified. PCA was used to establish the relationship between the origins and the volatile compounds for further discriminant analysis. The results showed that the PDMS/GO/DES method was a rapid, simple and sensitive technique for the analysis of volatile components in spices.
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ANALYTICAL LETTERS
·
2022
·
IF 2.267
Yimei Zeng,Changliang Ke,Qi Liu,Ke Huang
Organophosphate esters (OPEs) are commonly used in commercial products as flame retardants. In the present study, a simple method was established for the simultaneous determination of 10 OPEs in aquacultural water and sediments. The targets were extracted using dichloromethane or ethyl acetate, cleaned up by solid-phase extraction, and determined by gas chromatography – tandem mass spectrometry. The matrix effects were lower than 20% for all OPEs except for tris(2-chloroethyl) phosphate in sediments (matrix effect: 29.4%). In spiked water samples, the recoveries of the OPEs were from 72.3% to 108% with relative standard deviations ≤10.2% and the limits of detection from 0.17 to 1.13 ng·L−1. In spiked sediments, the recoveries of the OPEs were from 101% to 121% with relative standard deviations ≤11.2% with limits of detection from 0.02 to 0.32 ng·g−1, dry weight (dw). The developed method was applied to the analysis of aquaculture samples from Kaozhouyang Bay, China. The total concentration ranges of the 10 OPEs in the water and sediments were from 121 to 159 ng·L−1 and 7.54 to 13.3 ng·g−1, dw, respectively.
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FOOD CONTROL
·
2023
·
IF 6
Ziming Xie,Dequan Zeng,Jingwen Wang,Mouming Zhao,Yunzi Feng
In the present work, a dispersive liquid-liquid microextraction (DLLME) method combined with gas chromatography-mass spectrometry (GC-MS) was successfully developed for accurate determination of aroma-active components in soy sauce . Several key experimental parameters were optimized, including the type of dispersant, vortex time and the volume ratio of extractant and dispersant. The optimal conditions were 1200 μL acetone as dispersant, 800 μL dichloromethane as extractant and 3 min of vortex mixing. The proposed method was validated, achieving good linearities with R 2 ≥ 0.9941, recoveries between 82 and 129% with 4-hydroxy-2,5-dimethyl-3(2H)-furanone (HDMF) and 4-hydroxy-2 (or 5)-ethly-5 (or 2)-methyl-3(2H)-furanone (HEMF) within 84–103%, relative standard deviations ranging from 0.02 to 8.60% with HDMF and HEMF between 0.26 and 1.44%, and limits of detection and limits of quantification in the range of 0.08–35.95 μg/L and 0.25–119.83 μg/L, respectively. The entire sample processing with DLLME was completed in roughly 15 min with a total consumption of 2 mL of organic solvent, and 93 volatiles identified in the obtained extracts, with 87.1% (81 volatiles) showing relative standard deviations lower than 10%. Compared to conventional liquid-liquid extraction (LLE), DLLME exhibited obvious advantages of simplicity, rapidity, stability and low solvent consumption, favouring the extraction of acids and ketones. This is the first application of the DLLME technique for the analysis of aroma compounds in soy sauce and is suitable for rapid determination of key aroma compounds like HDMF and HEMF, especially for routine detection and large batch analysis of soy sauce, which can provide reliable information for soy sauce flavour analysis.
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2021
·
IF 4.556
Sam Al-Dalali,Fuping Zheng,Baoguo Sun,Talmizur Rahman,Feng Chen
Aging is an essential step for enriching the aroma profiles of Chinese vinegar. This study aimed to track the volatile flavor changes in the same batch of Chinese vinegar for the first time during two years of aging with the aid of HS-SPME-GC–MS. The aroma-active compounds were characterized at 0, 6, and 12 months of aging using GC-O coupled with a modified frequency method. A total of 67 volatile compounds and 30 aroma-active compounds were identified during the different stages of aging. Most alcohols, esters, ketones, acids, and phenols decreased during the aging from 628.4, 105.4, 132.1, 22.1, and 21.4 μg/L at 0 month to 228.7, 7.2, 9.69, 17.24, and 11.6 μg/L at 24 months separately, except aldehydes and pyrazines, which showed slight increases. Many aroma-active compounds were generated during the aging, such as methional, trimethylpyrazine, acetophenone, and 2-acetyl-3-ethylpyrazine, while pyrazines were formed during 24 months of aging. Three aroma-active compounds with high odor activity values (OAVs) showed significant contributions to the aroma profile of vinegar, which included isovaleric acid (2743, 340, and 3139), 4-ethylguaiacol (580, 429, and 516), and γ -nonalactone (324, 640, and 442) at 0, 6, and 12 months of aging, respectively.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2024
·
IF 5.7
Qing Zhang,Jiaping Ke,Piaopiao Long,Mingchun Wen,Zisheng Han,Liang Zhang,Mengting Zhu
The linoleic acid reaction models were set at 150 °C for 120 min, and its oxidation process was monitored by nuclear magnetic resonance (NMR) and gas chromatography–mass spectrometry (GC-MS). Results showed that no furan was formed from linoleic acid without heating, while furan accumulated throughout the heating process. Linoleic acid ran out within 30 min, which indicated that furan was formed mainly from the intermediate oxidation products of linoleic acid after 30 min. It should be noticed that the content of (E,E)-2,4-decadienal reached maximum once the linoleic acid ran out and then decreased with the formation of furan. Multivariate statistical analysis suggested that (E,E)-2,4-decadienal was the most important aldehyde related to furan formation during linoleic acid oxidation. To prove this assumption, the variation of furan from (E,E)-2,4-decadienal reaction models heating at 150 °C for 60 min was also studied. Results showed that the content of furan increased with the oxidation of (E,E)-2,4-decadienal. Furthermore, NMR and GC-MS data proved that (E,E)-2,4-decadienal could be oxidized to 4,5-epoxy-(E)-2-decenal. In conclusion, our results supported (E,E)-2,4-decadienal and trans-4,5-epoxy-(E)-2-decenal as critical intermediate products of furan formation from linoleic acid oxidation.
研究领域:
化学
·
食品科学
·
分析化学
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FOOD CHEMISTRY
·
2024
·
IF 8.5
Tianyu Ma,Chunguang Wang,Xinyue Zhang,Yuxuan Zhu,Jiani Liu,Jian Sun,Baoqing Zhu,Dongqing Ye
Two varieties of mango juices (MJs) were separately fermented with 40 strains Lactiplantibacillus plantarum . The volatile compounds and sensory characteristics of the fermented mango juices (FMJs) were analyzed by HS-SPME-GC–MS and Napping method. The results demonstrated well growth among all strains except for LC25. Strains SS6 and B15 demonstrated the strongest acid production capacity in ReNong and Ketti MJs. Seventy-five volatile compounds were identified, showcasing strain-specific differences. Fermentation significantly enhanced the complexity and intensity of aroma compounds, especially terpenes, esters and alcohols. Sensory evaluation categorized FMJs into six aroma profiles, with strains C10 and LA100 exhibiting pleasant ‘mango’ flavor in ReNong and Ketti MJs. Multivariate factor analysis revealed that esters potentially play a key role in enhancing the ‘mango’ and ‘floral’ aroma of the FMJs. This study serves as a valuable resource for Lp. plantarum strain selection and quality control in FMJ development by analyzing the acid and aroma diversity.
研究领域:
食品科学
·
微生物学
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分析化学
·
感官评价
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2018
·
IF 2.441
Xiaoyu Lu,Min Fang,Yu Dai,Yue Yang,Ali Fan,Jiaqiu Xu,Zhiying Qin,Yang Lu,Di Zhao,Xijing Chen,Ning Li
PEGylation techniques have been increasingly employed in drug delivery system and chemical modification of compounds with low aqueous solubility. Triacontanol (TA) is a natural product with several pharmacological activities, but its low aqueous solubility significantly limited its application. PEGylated triacontanol (PEG-TA) was designed as the prodrug to improve the aqueous solubility and pharmacokinetic properties of TA. On the basis of salting-out assisted liquid-liquid extraction (SALLE) and saponification sample preparation procedure, a reliable gas chromatography tandem mass spectrometric (GC–MS/MS) method was developed and validated for the quantification of PEG-TA and its metabolite TA in rat plasma after separation and transformation. Acetonitrile-methanol (9:1, v/v) and ammonium acetate (10 M) were utilized to separate PEG-TA and TA (including conjugated TA with fatty acid). Saponification facilitated the complete conversion of PEG-TA into TA, so PEG-TA could be indirectly quantified. The results revealed that the GC–MS/MS method had excellent selectivity, accuracy and linearity. Calibration curves were linear (R 2 >0.99) within the range of 20.0–1000.0 ng/mL for TA and 100.0–10,000.0 ng/mL for PEG-TA. The intra- and inter-day precision of quality control samples were within 15%, and their accuracy values varied from 93.54% to 113.38%. This analytical method has been successfully applied to pharmacokinetic study of PEG-TA. This study can facilitate the further exploration and quantification of PEGylated prodrugs.
研究领域:
药物化学
·
分析化学
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药理学
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Journal of Essential Oil Bearing Plants
·
2016
·
IF 0.313
Xin Chao Liu,Shao Liang Liu,Zhi Long Liu
In our screening program for new agrochemicals from wild plants and Chinese medicinal herbs, Teucrium quadrifarium aerial parts at flowering stage was found to possess strong insecticidal activity against booklice (Liposcelis bostrychophila). Water-distilled essential oil from T. quadrifarium aerial parts was analyzed by gas chromatography-mass spectrometry (GC-MS). Fourty-seven components comprising 97.2 % of the total oil were identified and the main components of the essential oil were germacrene D (8.8 %), linalool (8.2 %), camphene (7.8 %), β-caryophyllene (7.3 %), β-cadinene (6.8 %), 1,8-cineole (6.5 %), 4-terpineol (5.8 %), and α-terpineol (5.1 %). The essential oil of T. quadrifarium possessed contact toxicity against L. bostrychophila with a LC50 value of 95.1 μg/cm2. The oil also showed fumigant toxicity against L. bostrychophila with a LC50 value of 222.0 μg/l. These findings suggested that the essential oil of T. quadrifarium aerial parts has potential to be developed as new natural insecticides for the control of grain storage insects.
研究领域:
植物化学
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昆虫学
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农业科学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2025
·
IF 4.6
Tongtong Yang,Bo Tang,Junyi Tang,Chenqi Xu,Yanlong Hong,Fei Wu,Xiao Lin
Pheretima products are widely used, but the stenchy odor is a constraint to their application. In this study, 86 and 673 volatile components (VOCs) were identified in Pheretima and its extracts using headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS), respectively. An increase in acid and amine contents after processing was found, which may explain the increased stenchy odor. Through orthogonal partial least squares discriminant analysis (OPLS-DA), 14 differential markers between aqueous and alcoholic extracts were screened, and 3-methylbutanal, pentanal, and trimethylamine were identified as the key differential odor components. Combined with relative odor activity value (ROAV) analysis, 10 key odor components were identified, including: 3-methylbutanal, 1-octen-3-ol, dimethyl trisulfide, (2 E ,6 Z )-nona-2,6-dienal, methyl mercaptan, guaiacol, isobutyraldehyde, 1,8-cineole, 2-pentylfuran, and pentanal. This study provides theoretical support for the optimization of the odor of Pheretima-containing products and promotes their application.
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JOURNAL OF THE AMERICAN OIL CHEMISTS SOCIETY
·
2025
·
IF 2.4
Hongjie Zhang,Shengyan Zhang,Junyi Ma,Youqiong Liu,Xueli Chen,Weibao Kong,Ji Zhang
This study employed a complementary analytical approach, combining headspace gas chromatography–ion mobility spectrometry (HS-GC-IMS) and headspace gas chromatography–mass spectrometry (HS-GC-MS), to comprehensively characterize the dynamic evolution of volatile organic compounds (VOCs) in virgin olive oil (VOO) from Chenggu 32 (CG-32) and Koroneiki (KK) cultivars across eight maturity indices (MIs). The combined strategy proved powerful: HS-GC-IMS detected 90 VOCs, excelling in profiling polar, aroma-active compounds, while HS-GC-MS confirmed 61 VOCs, providing broader metabolome coverage. Multivariate statistical analysis revealed that genetic cultivar is the primary driver of VOCs profile divergence. The CG-32 variety was characterized by a high abundance of aldehydes, imparting classic “green” notes, whereas the KK variety was dominated by ketones, resulting in a less traditional, intense aroma. Notably, a key finding was that genetic factors can override ripening trends, as evidenced by the late-harvest KK sample clustering with the early-harvest CG-32 sample based on VOCs signature. Orthogonal partial least squares-discriminant analysis (OPLS-DA) models exhibited exceptional predictive power ( Q 2 > 0.94) for varietal authentication, and a set of 35 key discriminatory markers (VIP > 1.0) was identified. This work underscores that MIs alone is an insufficient harvest guide and establishes a robust foundational methodology for VOCs-based quality control and varietal screening of olive oils. The high predictive power of the models demonstrates their potential for authenticity purposes, which now warrants validation with a larger sample set. Graphical Mapping the aroma of virgin olive oil: A dual-technique approach. HS-GC-IMS/MS analysis of two cultivars across eight maturity stages uncovered 35 key VOCs dictating oil identity and maturation. Multivariate modeling enabled precise differentiation, establishing a novel method for quality and authenticity verification.
研究领域:
食品化学
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分析化学
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香气科学
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园艺科学
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代谢组学
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Huan Liu,Siyuan Di,Yunkang Liu,Zihan Li,Pin Chen,Shukui Zhu
A novel magnetic mesoporous fluorinated metal-organic framework material (Fe 3 O 4 @MIP-206-F) has been synthesized specifically for application as an adsorbent for perfluoroalkyl carboxylic acids (PFCAs) extraction by magnetic solid-phase extraction (MSPE). The carefully designed Fe 3 O 4 @MIP-206-F material features an appropriate porosity, open metal sites of Zr, and functional groups (fluorine and amino) conducive to the adsorption process. The distinctive architecture of the material endows it with exceptional extraction capabilities for PFCAs. Adsorption mechanisms encompass acid-base interactions, hydrophobic interactions, F-F interactions, electrostatic interactions, and size complementarity. Optimization of key parameters has significantly improved the extraction efficiency of MSPE. When coupled with gas chromatography-mass spectrometry (GC–MS), MSPE offers rapid and highly sensitive analysis of PFCAs. The method demonstrates wide linear range (0.050–50 ng mL −1 ), low detection limits (0.0010–0.0019 ng mL −1 ), good recoveries (86.7 % to 111 %), and exceptional intra- and inter-day precision. This approach accurately quantifies PFCAs in lake water and groundwater samples, enabling precise assessment of environmental contamination levels and supporting targeted remediation efforts.
研究领域:
环境科学
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分析化学
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JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS
·
2025
·
IF 6.2
Yande Cai,Ze Wang,Jianjun Wang,Songgeng Li
The formation of chloride products in the process for pyrolysis of municipal solid wastes (MSW) with key model components was investigated by Py-GC/MS method. HCl and CH 3 Cl are identified as the most abundant chloride products for the individual pyrolysis of polyvinyl chloride (PVC) or corn straw (CS) in the range of 200–600 °C. For the pyrolysis of CS, a higher temperature is more favorable for the generation of HCl than that of CH 3 Cl. In the PVC pyrolytic products, chlorobenzene (Ph-Cl), benzyl chloride (Ph-CH 2 Cl), and 1-(chloroethyl)benzene (Ph-CHClCH 3 ) are also detected but in extremely low amounts. For the co-pyrolysis of PVC/CS, the formation of CH 3 Cl is significantly promoted. The synergistic effect in the PVC/CS co-pyrolysis process is mainly attributed to the reaction between the HCl derived from PVC and the decomposition products of lignin. The products of Ph-Cl and Ph-CH 2 Cl are mainly generated from the cyclization of Cl-containing chain species. CH 3 Cl and Ph-CHClCH 3 are mainly generated from secondary reactions between HCl and other pyrolytic products. No remarkable synergistic effect is observed on the formations of chlorides in the co-pyrolysis of PVC/PP (polypropylene), while the generation of Ph-CHClCH 3 is significantly enhanced in the co-pyrolysis of PVC/PS (polystyrene).
研究领域:
环境科学
·
化学工程
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