CHROMATOGRAPHIA
·
2018
·Vol. 82
·期 3
·683-693
·
IF 1.401
Shen Chen,Wu Tong,Zang Xiaohuan
In this work, a zeolitic imidazolate framework-based graphene oxide composite (ZIF-8@GO) was prepared and used as the adsorbent in hollow fiber stir bar sorptive extraction. The stir bar was constructed of a small section of hollow fiber filled with 5 mg ZIF-8@GO and a thin stainless wire of 1.5 cm long in its lumen, and used to extract the trace levels of phthalate esters from children’s food samples prior to gas chromatography–mass spectrometric detection. The ZIF-8@GO showed a high adsorption efficiency for the compounds containing aromatic rings. The main experimental parameters that can impact the extraction efficiency including extraction temperature, extraction time, stirring rate, sample salinity, and desorption conditions were investigated. Under the optimized conditions, the limits of detection (LODs) for the five phthalate esters (diethyl phthalate, dipropyl phthalate, diisobutyl phthalate, butylbenzyl phthalate, and di(2-ethylhexyl) phthalate) were 0.15–0.6 µg L −1 for CiCi beverage and pear juice samples, and 0.75–2.2 µg kg −1 for jam samples. The limits of quantitation (LOQs) were 0.5–2.0 µg L −1 for CiCi beverage and pear juice samples, and 2.5–7.5 µg kg −1 for jam samples. Wide linear ranges of 0.5–500.0 µg L −1 and 2.5–2000 µg kg −1 were obtained for CiCi beverage, pear juice samples and jam samples, respectively, with good repeatability (RSD < 11%) and high method recoveries (72%–100%). The lifetime test results showed that the ZIF-8@GO-based hollow fiber stir bar can be reused for 120 extraction cycles without a significant loss of extraction efficiency, indicating its high durability and stability. The established method was applied successfully for the determination of the phthalate esters (PAEs) in children’s food samples. Graphical abstract
研究领域:
分析化学
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食品安全
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环境毒理学
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暴露科学
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食品化学
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污染物检测
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RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2026
·Vol. 40
·期 21
·e70164
·
IF 1.8
Jiale Fang,Zhijun Yuan,Yunfei Zhao,Lingling Teng,Lingxia An,Kezhi Jiang
Rationale Volatile methylcyclosiloxanes, particularly octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6), are commonly found in the environment and have gained significant attention as emerging contaminants. However, their accurate quantification at trace levels can be challenging because of complex environmental matrices and background interferences. Method VMCSs were extracted from water using vortex-assisted small-scale liquid–liquid extraction (LLE) with n -hexane as the extractant. Both the VMCS standards and the extracts were analyzed using gas chromatography–mass spectrometry (GC–MS). The mechanistic fragmentation of D4, D5, and D6 in EI-MS was studied through 13 C-labeling experiments. Results In EI-MS, the molecular ion readily eliminates a methyl radical to form the ion [M–CH 3 ] + for D4, D5, and D6. For D4, the ion [M–CH 3 ] + subsequently loses CH 4 , while the ions corresponding to D5 and D6 tend to undergo cyclization and methyl-shift, resulting in the characteristic ions of (CH 3 ) 3 Si + ( m/z 73) and [M–CH 3 –CH 4 ] + . These characteristic ions were used as the quantitative or qualitative indicators in the developed GC–MS method for determining D4, D5, and D6, achieving limits of quantification of 0.72–0.99 ng/mL. Efficient extraction of VMCSs in water was achieved within 12 min at room temperature, using only 0.40 mL of n -hexane for each extraction operation. Isotope-spiked experiments demonstrated satisfactory recoveries: 107.9% ± 8.0% for D4, 97.2% ± 5.8% for D5, and 84.7% ± 5.6% for D6. Analysis of real water samples revealed concentrations of D4, D5, and D6 in surface water ranging from 0.05 to 0.09 ng/mL, 0.07 to 0.27 ng/mL, and 0.07 to 0.25 ng/mL, respectively. Conclusion We developed a convenient and accurate method for the determination of trace level of D4, D5, and D6 in water, which addresses the limitations of traditional LLME, and offers a simple and environmentally friendly detection protocol for quantifying trace VMCSs in water.
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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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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2026
·
IF 6.7
Haiguang Tan,Lexuan Yang,Yunzhe Li,Xin Zhang,Tao Yang,Zhiguo Huang,Huan Zhang,Lijuan Ma,Lin Yuan,Liping Du
Abstract Quantitative GC-MS analysis of nonvolatile metabolites conventionally requires multisample external calibration, imposing substantial preparative overhead in high-throughput settings. Here, the integration of silylation derivatization with an isotopologue-based one-sample calibration curve (OSCC) on GC-MS platforms is reported. Trimethylsilylation introduces silicon atoms with invariant natural isotope abundances (28Si:29Si:30Si = 92.23%:4.68%:3.09%), enabling multiple calibration anchors from a single standard injection. Two strategies were developed: OSCC with multiple isotopologue selected ion monitoring (OSCC-MISM) on GC-MS, serving as a compositional-verification precursor, and OSCC with multiple isotopologue reaction monitoring (OSCC-MIRM) on GC-MS/MS, recommended for real-sample quantification. Both were validated against multisample calibration curve (MSCC)-SIM and MSCC-MRM across 12 nonvolatile organic acids, achieving R2 > 0.99, RSDs below 16.1%, and recoveries of 80.5–111.2%. In 15 commercial Baijiu samples, Bland–Altman analysis of 180 paired measurements gave a pooled bias of +0.8%, with 95% limits of agreement within the prespecified ±15% margin, supporting equivalence of OSCC-MIRM with MSCC-MRM.
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MOLECULES
·
2025
·Vol. 30
·期 7
·1404
·
IF 4.6
Qingling Xie,Hanwen Yuan,Shiqi Liu,Ling Liang,Jiangyi Luo,Mengyun Wang,Bin Li,Wei Wang
Forsythia suspensais a crucial plant resource due to its considerable edible and medicinal value. Its fruit, named Forsythiae Fructus (FF), has been widely used in Traditional Chinese Medicine (TCM). According to the fruit maturity stage, FF is categorized into GFF (green Forsythiae Fructus) and RFF (ripe Forsythiae Fructus). In this study, metabolomics based on UPLC-Q/Orbitrap MS and HS-GC-MS, combined with chemometric methods, was employed to differentiate GFF from RFF and identify potential differential metabolites. Additionally, the mid-level data fusion method was employed to integrate data from both techniques, and the performance of the OPLS-DA model (R2Y = 0.986, Q2= 0.974) surpassed that of the single HS-GC-MS technique (R2Y = 0.968, Q2= 0.930). Moreover, using the criteria of VIP > 1 andp-value < 0.05, 30 differential compounds were selected via mid-level data fusion, compared to the initial 61 differential compounds identified by single techniques, effectively reducing data noise and eliminating irrelevant variables. This study provides a comprehensive analysis of volatile and non-volatile compounds in FF, offering valuable insights into quality control and clinical differentiation between GFF and RFF. The findings highlight the potential use of multi-technology metabolomics in the quality control of TCM and offer new perspectives for future research on medicinal plants.
研究领域:
中药学
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分析化学
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CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
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2024
·
IF 1.2
Qinghua YANG,Zhimin HE,Yilan SHI,Jinxin WANG,Qianying QIU,Honghai DENG,Wenhui PING
In this study, a new technique was developed which combines magnetic solid phase extraction (MSPE) and gas chromatography-mass spectrometer (GC–MS), for the analysis of 17 phthalate esters (PAEs). First, a composite of iron (used as the magnetic part) and graphene oxide (GO) was synthesized for application in MSPE. Scanning electron microscop, X-ray diffraction and infrared spectroscopy were used to characterize this material. Finally, magnetic graphene oxide (Fe₃O₄@GO) was used to extract PAEs from water samples. Various parameters relevant to the extraction were optimized, such as the amount of adsorbent employed, adsorption time, luent solvent types and volume, and sample pH. These optimum conditions resulted in calibration curves for the 17 PAEs, showing linear relationships between concentration and response at concentrations of 25 to 2500 µg L⁻¹ with correlation coefficients from 0.9983 to 1.000. Limit of detection and limit of quantitationfor the PAEs ranged from 0.030 to 0.12 µg L⁻¹ and 0.10–0.40 µg L⁻¹, respectively. The recovery rates for these compounds in spiked samples were ranging from 81.5% to 109% with relative standard deviation less than 6.12%. The effectiveness of method was further demonstrated by its use in detecting 17 PAEs in samples of drinking and bottled water. Compounds such as DEP, DIBP, DBP, and DCHP were identified. These results thus highlight the suitability of Fe₃O₄@GO as an adsorbent for concentrating and purifying PAEs in water samples.
研究领域:
环境科学
·
分析化学
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Yuan Yang,Xiaoli Wu,Qiuyi Yan,Hongling Zhou,Yurong Deng,Chengbin Zheng
Furans, recognized as carcinogenic contaminants generated during thermal food processing, pose significant food safety concerns, necessitating sensitive and cost-effective detection methods. Traditional GC-FID/MS methods are often constrained by high costs and complex instrumentation. Herein, a point discharge molecular emission spectrometer (PD-MES) was developed as a highly sensitive GC detector, specifically by monitoring CN molecular emission at 388.3 nm for the analysis of furans in food samples. Furans were extracted using headspace solid-phase microextraction (HS-SPME) prior to detection. Compared to conventional carbon atomic emission at 193.0 nm, the CN-based method demonstrated up to a 211.42-fold improvement in sensitivity and achieved detection limits of 0.02–0.08 ng/g with excellent precision (RSD < 4.9 %). Practical validation across ten diverse food matrices yielded satisfactory recoveries (83.4 %–114.5 %). This system offers a robust, highly sensitive, reliable, and economical alternative for the routine monitoring of furan compounds in foods, particularly in resource-limited settings.
研究领域:
食品安全
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分析化学
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光谱学
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环境卫生
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毒理学
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PubMed
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FOOD RESEARCH INTERNATIONAL
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2025
·
IF 8
Sihui Guan,Fei Yang,Jinxiao Yao,Chaochao Liu,Rongqing Wang,Meiying Ruan,Zhuping Yao,Chenxu Liu,Hongjian Wan,Zhimiao Li,Ming Diao,Yuan Cheng
Cherry tomatoes are widely appreciated for their distinctive taste and aroma. To explore the impact of low temperatures on the quality and flavor of ripe red tomatoes, this study examined changes in the volatile organic compounds (VOCs) in fruits stored at 4 °C and 25 °C using headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS). A flavor fingerprint was developed using topographic plots, identifying 75 VOCs predominantly associated with aldehydes, ketones, alcohols, esters, and other compounds such as acids, sulfides, and furans. During storage at 4 °C, the primary volatile compounds identified were 6-methyl-5-hepten-2-one, butanol, and 1-penten-3-ol. In contrast, at 25 °C, 2-hexenal, hexanal, and acetic acid were the predominant compounds. Notably, storage at 25 °C was more effective in preserving the C6 aldehydes, which are known for their fresh, green, fatty, fruity, and sweet aromas. Principal component analysis (PCA) and fingerprint similarity analysis (FSA) clearly differentiated the samples based on their storage temperature and duration, highlighting significant shifts in the flavor profile over time. Additionally, heat map clustering analysis supported the PCA results, further revealing differences and similarities among the samples. The study found that storage at 4 °C helped maintain the sensory quality, color, firmness, and soluble solids content (SSC) of the cherry tomatoes harvested at the red ripe stage. Significant correlations between fruit quality traits and certain VOCs suggest that key physicochemical indicators are closely tied to aroma compound dynamics during storage. However, the content of most VOCs decreased under refrigeration, indicating a reduction in flavor complexity at low temperatures. These findings contribute valuable insights into how storage conditions influence the flavor profile of cherry tomatoes and may guide optimization of postharvest storage protocols to balance quality retention and flavor preservation.
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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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Algal Research-Biomass Biofuels and Bioproducts
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2026
·
IF 5
Jikang Sui,Jinku Zhang,Xiangning Lu,Kangning Wang,Mingkai Bai,Adewale Olusegun Obadina,Shiyang Li,Guangxin Feng,Haohao Wu
Microalgae are a sustainable and nutrient-dense food source, but their strong off-flavors significantly limit broader consumption. This study evaluates the effectiveness of a laccase-catechin mediator in improving the odor profiles of Spirulina, Chlorella, and Chlamydomonas reinhardtii . Mediators were applied ex situ (pre-formed) or in situ (generated within the suspension). Ex-situ mediators, optimized at 40 °C for 2 h, achieved better deodorization compared to in-situ mediators, with optimal catechin dosages of 28, 16, and 8 mg/g biomass for Spirulina, Chlorella, and C. reinhardtii , respectively. Sensory evaluation showed reduced grassy, earthy, and fatty odors, and enhanced floral and fruity notes, with the ex-situ approach leading to higher overall acceptability. GC–MS analysis confirmed that mediators decreased the diversity and abundance of key odor-active volatiles in three microalgae species. Laccase-catalyzed quinone-type mediators effectively neutralize undesirable compounds, offering a promising enzymatic strategy for improving the sensory quality of microalgae-based foods, especially for sustainable food applications.
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MOLECULES
·
2026
·Vol. 31
·期 5
·
IF 5.1
Jing Sun,Yu Zhang,Hao Zhang,Rui Chen,Lin Zhang,Fengmao Liu,Xiaofeng Xue
Royal jelly, a nutrient-rich bee product characterized by high water content and active components, is particularly susceptible to quality deterioration during storage. While temperature effects have been extensively documented, the specific role of light exposure in quality degradation remains largely unexplored. despite its relevance during production, handling, transportation, and display. This study systematically investigated the volatile organic compounds (VOCs) of royal jelly under different storage conditions using gas chromatography-ion mobility spectrometry (GC-IMS) combined with fingerprint analysis. Results from dual-column validation demonstrated that even short-term light exposure at 25 °C induced pronounced alterations in VOC profiles, triggering the accumulation of off-flavor aldehydes (e.g., hexanal, nonanal) and ketones, along with 2-furfural generated via Maillard reaction. Concurrently, characteristic fresh-aroma esters and alcohols were significantly depleted. Multivariate statistical analysis confirmed light exposure as the predominant factor driving quality deterioration, with temperature variation under dark conditions producing comparatively minor effects within the same short timeframe. This work provides the first systematic evidence establishing insights into early volatile changes in royal jelly and identifies key VOC markers that offer valuable insights for optimizing storage strategies and developing rapid quality monitoring protocols.
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TALANTA
·
2013
·
IF 3.498
Shasha Zhao,Mian Wu,Faqiong Zhao,Baizhao Zeng
A novel polyaniline–polypyrrole (PANI–PPY) composite film coated stainless steel wire was prepared by cyclic voltammetry. Firstly, PANI was electrodeposited on a stainless steel wire from a solution containing 0.1 M aniline and 1 M HNO 3 , after the PANI coating was dried in air PPY was electrodeposited on it from a solution containing 0.1 M pyrrole and 0.1 M p -methylbenzene sulfonic acid. The resulting PANI–PPY fiber showed reticulate structure and had large specific surface area. When it was used for the headspace solid-phase microextraction of several esters (i.e. methyl anthranilate, ethyl-o-aminobenzoate, dimethyl phthalate, methyl laurate, and diethyl phthalate), followed by gas chromatographic determination, it presented higher extraction capability in comparison with PPY and PANI coatings. Under the optimized conditions, the linear ranges were 0.07−300 μg L −1 and the detection limits were 0.05−0.38 μg L −1 for different esters. The PANI–PPY fiber also showed high durability, after being used for about 160 times its extraction capacity only changed a little. The proposed method was successfully applied to the determination of these esters in real samples and the recoveries were 90–102%.
研究领域:
分析化学
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材料科学
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电化学
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环境分析
·
分离科学
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危险品化学品经营许可证（带存储）