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RSC Advances · 2018 ·Vol. 8 ·期 69 ·39641-39649 · IF 2.936

Magnetic solid-phase extraction using a mixture of two types of nanoparticles followed by gas chromatography-mass spectrometry for the determination of six phthalic acid esters in various water samples

Hui Li,Zhen Cao,Xiaolin Cao,Zejun Jiang,A. M. Abd El-Aty,Yan Qi,Hua Shao,Fen Jin,Lufei Zheng,Jing Wang

Two types of magnetic microspheres (Fe3O4@MIL-100 and Fe3O4@SiO2@polythiophene) were prepared and characterized as mixed sorbents for magnetic solid-phase extraction (MSPE) of six phthalic acid esters (PAEs), including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP), and di-n-octyl phthalate (DnOP) from water samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. The synthetic magnetic nanocomposites exhibited good repeatability and chemical stability, and improved extraction efficiency for the tested PAEs. The mixture of the two types of nanoparticles substantially improved the extraction efficiency of both DMP and DEP. The key parameters affecting the extraction efficiency, such as the type and the amount of sorbent, eluent (desorption solvent), adsorption and desorption time, pH of sample solution, and sample volume, were investigated and optimized, respectively. Under optimized conditions, the developed method showed satisfactory linearity in the range of 5–5000 μg L−1 with coefficients of determination (R2) > 0.9935. The method detection limits (MDLs) and limits of quantitation (LOQs) were between 0.35–0.91 μg L−1 and 1.1–2.9 μg L−1, respectively. At three fortification levels (1.0, 10.0, and 50.0 μg L−1), the mean recoveries ranged from 76.9–109.1% with favorable relative standard deviations (RSDs) < 9%. The feasibility of the method was evaluated by analysis of water samples from various sources (tap, drinking, and mineral water). The results show that the developed method is suitable for determination of trace level PAEs in water samples.

CAS / MDL: 79-41-4 110-02-1 78-10-4
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2016 · IF 2.687

Simultaneous determination of six short-chain fatty acids in colonic contents of colitis mice after oral administration of polysaccharides from Chrysanthemum morifolium Ramat by gas chromatography with flame ionization detector

Jin-hua Tao,Jin-ao Duan,Shu Jiang,Jian-ming Guo,Yi-yun Qian,Da-wei Qian

Short-chain fatty acids (SCFAs) produced by the intestinal bacteria are very critical for the intestinal barrier, mucosal cytoprotection and normal intestinal biology. However, accumulation of SCFAs promoted by the polysaccharides from Chrysanthemum morifolium Ramat remains unknown. Thus, it is necessary to investigate SCFAs in the colonic contents of dextran sulfate sodium (DSS) induced colitis mice after oral administration of the polysaccharides from C. morifolium Ramat which is very helpful to unravel how it works. In this study, a rapid and reliable gas chromatographic method with flame ionization detector (GC-FID) for simultaneous determination of six SCFAs such as acetic acid (AA), propionic acid (PA), butyric acid (BA), isobutyric acid (IBA), valeric acid (VA) and isovaleric acid (IVA) has been developed and validated. Under the optimized chromatographic conditions and sample extraction procedure, good separation for 6 target compounds was obtained on a HP-INNOWAX column within 12   min. Results revealed that polysaccharides from C. morifolium Ramat positively affected the SCFAs intestinal production. The polysaccharides group had greater SCFAs concentration in colonic content than the DSS-treated group (P   <   0.05), which was decreased remarkably compared to the normal group (P   <   0.01). With the decrease of the polysaccharides dosage, the contents of AA, PA and VA increased gradually, while the change of BA concentration was the opposite. There was no significant difference in the content of IBA at the different administration concentrations. And the content of IVA reached the highest concentration 0.953   mg/g at lower dose of the polysaccharides. Additionally, oral administration of the polysaccharides prominently attenuated the body weight loss, reduced the disease activity index, rectal bleeding and stool consistency, improved colon shortening and macroscopic score of colitis. Our results indicated that the polysaccharides of C. morifolium Ramat might be used as prebiotic agents to prevent gut dysbiosis and inflammatory bowel disease.

CAS / MDL: 64-19-7 79-31-2 109-52-4
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PHYTOCHEMICAL ANALYSIS · 2024 · IF 3

A strategy to distinguish similar traditional Chinese medicines by liquid chromatography–mass spectrometry, electronic senses, and gas chromatography–ion mobility spectrometry: Marsdeniae tenacissimae Caulis and Paederiae scandens Caulis as examples

Jia-Wei Wang,Zhi-Dong Pei,Yue-Hua Chen,Si-Yu Li,Tian-Min Wang,Ting-Guo Kang,Na Li,Ya-Mei Song,Hui-Peng Song,Hui Zhang

Introduction Marsdeniae tenacissimae Caulis (MTC), a popular traditional Chinese medicine, has been widely used in the treatment of tumor diseases. Paederiae scandens Caulis (PSC), which is similar in appearance to MTC, is a common counterfeit product. It is difficult for traditional methods to effectively distinguish between MTC and PSC. Therefore, there is an urgent need for a rapid and accurate method to identify MTC and PSC. Objectives The aim is to distinguish between MTC and PSC by analyzing the differences in nonvolatile organic compounds (NVOCs), taste, odor, and volatile organic compounds (VOCs). Methods Liquid chromatography–mass spectrometry (LC-MS) was utilized to analyze the NVOCs of MTC and PSC. Electronic tongue (E-tongue) and electronic nose (E-nose) were used to analyze their taste and odor respectively. Gas chromatography–ion mobility spectrometry (GC-IMS) was applied to analyze VOCs. Finally, multivariate statistical analyses were conducted to further investigate the differences between MTC and PSC, including principal component analysis, orthogonal partial least squares discriminant analysis, discriminant factor analysis, and soft independent modeling of class analysis. Results The results of this study indicate that the integrated strategy of LC-MS, E-tongue, E-nose, GC-IMS, and multivariate statistical analysis can be effectively applied to distinguish between MTC and PSC. Using LC-MS, 25 NVOCs were identified in MTC, while 18 NVOCs were identified in PSC. The major compounds in MTC are steroids, while the major compounds in PSC are iridoid glycosides. Similarly, the distinct taste difference between MTC and PSC was precisely revealed by the E-tongue. Specifically, the pronounced bitterness in PSC was proven to stem from iridoid glycosides, whereas the bitterness evident in MTC was intimately tied to steroids. The E-nose detected eight odor components in MTC and six in PSC, respectively. The subsequent statistical analysis uncovered notable differences in their odor profiles. GC-IMS provided a visual representation of the differences in VOCs between MTC and PSC. The results indicated a relatively high relative content of 82 VOCs in MTC, contrasted with 32 VOCs exhibiting a similarly high relative content in PSC. Conclusion In this study, for the first time, the combined use of LC-MS, E-tongue, E-nose, GC-IMS, and multivariate statistical analysis has proven to be an effective method for distinguishing between MTC and PSC from multiple perspectives. This approach provides a valuable reference for the identification of other visually similar traditional Chinese medicines.

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JOURNAL OF SEPARATION SCIENCE · 2016 ·Vol. 39 ·期 18 ·3578-3585 · IF 2.741

Novel method for the rapid and specific extraction of multiple β2-agonist residues in food by tailor-made Monolith-MIPs extraction disks and detection by gas chromatography with mass spectrometry

Haibo Liu,Ning Gan,Yinji Chen,Qingqing Ding,Jie Huang,Saichai Lin,Yuting Cao,Tianhua Li

A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C 18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C 18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H 2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018–0.022 and 0.042–0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β 2 -agonists residues in real food samples.

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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2025 · IF 6.2

New Method of Direct Sampling Gas Chromatography–Ion Mobility Spectrometry to Identify the Dynamic Retronasal Volatile Compounds in the Alcoholic Beverage and Their Release Behaviors: A Case Study on Huangjiu

Yiwen Wang,Zhilei Zhou,Rui Chang,Zhimin Zhang,Xibiao Xu,Yuezheng Xu,Jian Mao

Owing to extremely low concentrations and dynamic changes, it is difficult to detect and trace the retronasal volatile organic compounds (VOCs) generated during the consumption of alcoholic beverages. We developed a direct sampling gas chromatography–ion mobility spectrometry (GC-IMS) method to identify the dynamic VOCs after drinking Huangjiu-a fermented alcoholic beverages. The optimal procedure was obtained: take a sip of 10 mL Huangjiu, holding it in mouth for 10 s and then swallow, and the VOCs in one nasal expiration were collected with gas sampling bag and transferred directly to the injection port of GC-IMS. The repeatability was satisfactory (RSD < 5%). Twenty-two VOCs were detected in Huangjiu, with esters and alcohols being dominant, which were divided into five distinct release behavior groups. Their release was found significantly inhibited by saliva. Overall, this new method offers a technical approach to understanding and assessing the characteristics of retronasal aroma in alcoholic beverages.

✓ 已验证 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2015 · IF 3.391

Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography–olfactometry (HS-SPME–GC–O): Altering sample amount, diluting the sample or adjusting split ratio?

Yunzi Feng,Yu Cai,Dongxiao Sun-Waterhouse,Chun Cui,Guowan Su,Lianzhu Lin,Mouming Zhao

Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography–olfactometry (GC–O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME–AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone.

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TALANTA · 2016 · IF 4.035

Simultaneous extraction and determination of phthalate esters in aqueous solution by yolk-shell magnetic mesoporous carbon-molecularly imprinted composites based on solid-phase extraction coupled with gas chromatography–mass spectrometry

Rui Yang,Yuxin Liu,Xiangyang Yan,Shaomin Liu

A rapid, sensitive and accurate method for the simultaneous extraction and determination of five types of trace phthalate esters (PAEs) in environmental water and beverage samples using magnetic molecularly imprinted solid-phase extraction (MMIP–SPE) coupled with gas chromatography–mass spectrometry (GC–MS) was developed. A novel type of molecularly imprinted polymers on the surface of yolk-shell magnetic mesoporous carbon (Fe 3 O 4 @void@C–MIPs) was used as an efficient adsorbent for selective adsorption of phthalate esters based on magnetic solid–phase extraction (MSPE). The real samples were first preconcentrated by Fe 3 O 4 @void@C–MIPs, subsequently extracted by eluent and finally determined by GC–MS after magnetic separation. Several variables affecting the extraction efficiency of the analytes, including the type and volume of the elution solvent, amount of adsorbent, extraction time, desorption time and pH of the sample solution, were investigated and optimized. Validation experiments indicated that the developed method presented good linearity (R 2 >0.9961), satisfactory precision (RSD<6.7%), and high recovery (86.1–103.1%). The limits of detection ranged from 1.6   ng/L to 5.2   ng/L and the enrichment factor was in the range of 822–1423. The results indicated that the novel method had the advantages of convenience, good sensitivity, and high efficiency, and it could also be successfully applied to the analysis of PAEs in real samples.

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ANALYTICA CHIMICA ACTA · 2024 · IF 5.7

Simple and sensitive monitoring of polycyclic aromatic hydrocarbons in edible oils by polydimethylsiloxane/pyrazine-based hyper-crosslinked polymer coated stir bar sorptive extraction followed by gas chromatography-mass spectrometry detection

Yiwen Han,Aikun Han,Yaqiong Qin,Yuan Tian,Bin Peng,Lijun He,Wenfen Zhang,Wenjie Zhao,Shusheng Zhang

Background Edible oils are susceptible to contamination with polycyclic aromatic hydrocarbons (PAHs) throughout production, storage, and transportation processes due to their lipophilic nature. The necessity of quantifying PAHs present in complex oil matrices at trace levels, which bind strongly to impurities in oil matrices, poses a major challenge to the accurate quantification of these contaminants. Therefore, the development of straightforward and effective methods for the separation and enrichment of PAHs in oil samples prior to instrumental analysis is paramount to guaranteeing food safety. Results A pyrazine embedded hyper-crosslinked porous polymer, HCP Pz-TPB , was synthesized via a Friedel-Crafts reaction, utilizing triphenylbenzene (TPB) as the monomer and 2,5-dibromomethylpyrazine as the cross-linking reagent. The material was combined with polydimethylsiloxane (PDMS) using the sol-gel method, and applied as a coating to a dumbbell-shaped stir bar prepared in-house. Using stir bar sorptive extraction (SBSE) combined with gas chromatography-mass spectrometry (GC-MS), 15 PAHs in edible oils were successfully quantified. Optimal conditions for the extraction of PAHs were experimentally investigated, with factors such as stirring rate, extraction time, extraction temperature, desorption solvent, and desorption time systematically optimized. The final method demonstrated a broad linear range (0.12–150 ng g −1 ), and low limits of detection (0.04–0.28 ng g −1 ). The recoveries of PAHs in real edible oil samples ranged from 83.14 % to 128.01 %, with relative standard deviations (RSDs) below 13.47 %. Significance This method simplifies PAH extraction by eliminating steps such as saponification, liquid-liquid extraction, drying, and re-dissolution, thus reducing potential analyte loss and errors associated with the inclusion of multiple pretreatment steps typical of conventional methods reported in the literature. Notably, the adsorbent materials prepared in this study can be reused up to 30 times, underscoring its sustainability. The proposed research broadens the diversity of coating choices for SBSE applications while offering a streamlined, cost-effective, and greener alternative for PAH determinations in edible oils via SBSE/GC-MS.

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INORGANIC CHEMISTRY · 2023 · IF 4.6

H2/D2 Separation Using UTSA-16@CAU-10-H@γ-AlOOH Composites as the Stationary Phase in Gas Chromatography via the Additive Effects of Kinetic Sieving and Chemical Affinity Quantum Sieving

Enming Ping,Xiaoxiao Chen,Yunshan Zhou,Lijuan Zhang,Lingyun Kong,Nan Chen

In this work, CAU-10-H@γ-AlOOH is prepared, and then UTSA-16 is loaded on CAU-10-H@γ-AlOOH to obtain UTSA-16@CAU-10-H@γ-AlOOH. Using the as-prepared composites as stationary materials by cryogenic gas chromatography at 77 K, while CAU-10-H@γ-AlOOH achieves the complete separation of ortho-H2 (o-H2) and D2 with a resolution R of 1.66 and a separation time t of 9.52 min, UTSA-16@CAU-10-H@γ-AlOOH achieves higher efficiency separation of hydrogen isotopes in a shorter separation time (4.56 min) with R = 1.7. Molecular simulation results show that CAU-10-H has both chemical affinity quantum sieving and kinetic sieving effects for H2/D2 at 77 K, and UTSA-16 can only exert the kinetic sieving effect. UTSA-16’s load on CAU-10-H@γ-AlOOH weakens the adsorption of hydrogen isotopes, and the presence of Co2+ in UTSA-16 promotes the conversion of para-H2 to ortho-H2. In gas chromatography, H2 was preferentially desorbed from the system due to strong D2 adsorption caused by the chemical affinity quantum sieving effect and faster H2 diffusion caused by the kinetic sieving effect. These additive effects achieved efficient hydrogen isotope separation at 77 K.

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Fermentation-Basel · 2021 ·Vol. 7 ·期 4 ·309 · IF 3.975

Co-Treatment with Single and Ternary Mixture Gas of Dimethyl Sulfide, Propanethiol, and Toluene by a Macrokinetic Analysis in a Biotrickling Filter Seeded with Alcaligenes sp. SY1 and Pseudomonas Putida S1

Yiming Sun,Xiaowei Lin,Shaodong Zhu,Jianmeng Chen,Yi He,Yao Shi,Hua Liu,Lei Qin

The biotrickling filter (BTF) treatment is an effective way of dealing with air pollution caused by volatile organic compounds (VOCs). However, this approach is typically used for single VOCs treatment but not for the mixtures of VOC and volatile organic sulfur compounds (VOSCs), even if they are often encountered in industrial applications. Therefore, we investigated the performance of BTF for single and ternary mixture gas of dimethyl sulfide (DMS), propanethiol, and toluene, respectively. Results showed that the co-treatment enhanced the removal efficiency of toluene, but not of dimethyl sulfide or propanethiol. Maximum removal rates (rmax) of DMS, propanethiol and toluene were calculated to be 256.41 g·m−3·h−1, 204.08 g·m−3·h−1and 90.91 g·m−3·h−1, respectively. For a gas mixture of these three constituents,rmaxwas measured to be 114.94 g·m−3·h−1, 104.17 g·m−3·h−1and 99.01 g·m−3·h−1, separately. Illumina MiSeq sequencing analysis further indicated that Proteobacteria and Bacteroidetes were the major bacterial groups in BTF packing materials. A shift of bacterial community structure was observed during the biodegradation process.Keywords:biotrickling filter;decomposition;dimethyl sulfide;pollution;propanethiol;toluene

CAS / MDL: 108-88-3
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FOOD RESEARCH INTERNATIONAL · 2020 · IF 4.972

Aroma dynamic characteristics during the process of variable-temperature final firing of Congou black tea by electronic nose and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry

Yanqin Yang,Jinjie Hua,Yuliang Deng,Yongwen Jiang,Michael C. Qian,Jinjin Wang,Jia Li,Mingming Zhang,Chunwang Dong,Haibo Yuan

The drying technology is crucial to the quality of Congou black tea. In this study, the aroma dynamic characteristics during the variable-temperature final firing of Congou black tea was investigated by electronic nose (e-nose) and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS). Varying drying temperatures and time obtained distinctly different types of aroma characteristics such as faint scent, floral aroma, and sweet fragrance. GC × GC-TOFMS identified a total of 243 volatile compounds. Clear discrimination among different variable-temperature final firing samples was achieved by using partial least squares discriminant analysis (R2Y = 0.95, Q2 = 0.727). Based on a dual criterion of variable importance in the projection value (VIP > 1.0) and one-way ANOVA ( p < 0.05 ), ninety-one specific volatile biomarkers were identified, including 2,6-dimethyl-2,6-octadiene and 2,5-diethylpyrazine with VIP > 1.5. In addition, for the overall odor perception, e-nose was able to distinguish the subtle difference during the variable-temperature final firing process.

CAS / MDL: 3081-61-6
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Food Analytical Methods · 2019 ·Vol. 12 ·期 5 ·1160-1169 · IF 2.413

Molecularly Imprinted Polymers with Dual Template and Bifunctional Monomers for Selective and Simultaneous Solid-Phase Extraction and Gas Chromatographic Determination of Four Plant Growth Regulators in Plant-Derived Tissues and Foods

Wang Chengjun,Ding Chuyuan,Wu Qiwei,Xiong Xiyao

A highly selective and sensitive molecularly imprinted polymer (MIP)-based solid-phase extraction (SPE) combined with gas chromatographic (GC) detection method was developed for the simultaneous isolation and determination of four plant growth regulators (PGRs) including indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), 1-naphthaleneacetic acid (NAA), and 2,4-dichlorophenoxyacetic acid (2,4-D) in plant tissues, fruits, and vegetables. The MIP composites, synthesized by application of dual template molecules (IAA and 2,4-D) and bifunctional monomers β -cyclodextrin ( β -CD) and methacrylic acid (MAA), were characterized by FTIR, BET, XRD, SEM, and TGA techniques. The effects of the amount of adsorbent, sample pH, and eluent solvents on the SPE performance were investigated. Under the optimal SPE condition, the β -CD/MAA-MIPs exhibited higher selective capability and greater adsorption capacity toward target PGRs when compared with commercial SPE adsorbents, single template, and functional monomer MIPs. In addition, the stability and reusability studies demonstrated that the synthesized β -CD/MAA-MIPs were capable for reutilization with stable performance in sample pretreatment process. Finally, the proposed β -CD/MAA-MIPs-SPE-GC technique was successfully applied to analyze the interested PGRs in different plant tissues, fruits, and vegetable samples.

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