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FOOD CHEMISTRY · 2023 · IF 8.8

Aroma characteristics of flaxseed milk via GC–MS-O and odor activity value calculation: Imparts and selection of different flaxseed varieties

Yang Yue,Chao Wang,Yashu Chen,Mingming Zheng,Yi Zhang,Qianchun Deng,Qi Zhou

Currently, the effect of varieties on the flavor and stability of flaxseed milk remains unknown. Therefore, this study was conducted to investigate the effects of different varieties on the stability, sensory, and aromas of flaxseed milk. 51 volatile compounds were identified in flaxseed milk using Stir Bar Sorptive Extraction-Gas Chromatography-Olfactometry-Mass Spectrometry (SBSE-GC-O-MS). Among them, 1-octen-3-ol, 2-methoxy-4-vinylphenol, and 2,3,5-trimethylpyrazine contributed higher relative odor active values (ROAV), resulted in the fruity, roasted, sweet, and cucumber in flaxseed milk. Isovaleraldehyde (green notes) was not detected in XHZM. However, other compounds such as 1-nonanol (floral), γ-nonanolactone and γ-octanoic lactone (coconut milk) had higher concentrations, causing a better sensory evaluation. Additionally, its stability was relatively good. The orthogonal partial least-squares regression (OPLS) model and VIP values showed that eight compounds were responsible for the sensory differences from different varietals. The study provided references to selection and understanding flavor composition basis of flaxseed milk.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Room-temperature synthesis of magnetic thiophene-based covalent organic frameworks for derivatization-assisted GC–MS analysis of estrogens in environmental water

Yue Bao,Yixin Zhai,Siyuan Di,Hailan Qin,Shukui Zhu

Under room temperature conditions, a novel thiophene-based magnetic covalent organic framework (COF) was ingeniously synthesized for the first time, utilizing an uncomplicated and benign Schiff base reaction between 4,4′,4″,4‴-(pyrene-1,3,6,8-tetrayl)tetraaniline (PyTTA) and 2,2′-dithiophene-5,5′-dicarboxaldehyde (BTDA), with Fe 3 O 4 serving as the magnetic nucleus. The fabricated Fe 3 O 4 @Py-BTDA COF nanocomposite displays superior crystallinity, homogenous pore size distribution, elevated magnetic responsiveness, and extraordinary thermal and chemical stability, which is an ideal sorbent for magnetic solid phase extraction (MSPE) of estrogens in environmental water samples. The presence of thiophene groups within the Fe 3 O 4 @Py-BTDA COF significantly bolsters the π-π interaction between the COF and the target analytes, and meanwhile provides sufficient hydrophobic sites and unique p-π interactions, thus becoming a crucial factor in augmenting the extraction efficiency of estrogens. Due to the high boiling point of estrogens, derivatization is necessary before gas chromatography–mass spectrometry (GC–MS) analysis. So, the conditions of derivatization, extraction and desorption were then systematically optimized. Under the optimal MSPE conditions, a rapid and sensitive method coupling MSPE with GC–MS was developed for the analysis of five estrogens in environmental water samples. The method showed good linearity (r 2  > 0.9997) in the range of 0.05–100 μg L −1 , low detection limits (4.0–7.0 ng/L), good spiked recoveries (91.56 %-105.80 %), and satisfactory relative standard deviations (RSD, less than 7.4 %). In addition, the method was successfully applied to the determination of estrogens in Yangtze River water, East Lake water, and tap water, with the recoveries in the range of 81.33 %-113.95 % and the RSDs in the range of 0.12 % to 7.69 % at different spiked levels. Estrone (E1) and estradiol (E2) were detected in the Yangtze River water with concentrations of 0.31 μg L −1 and 0.08 μg L −1 . And, the prepared Fe 3 O 4 @Py-BTDA COF nanocomposite still provides good extraction effect after five cycles of application. The developed method is rapid, simple, sensitive, and environmentally friendly, and has good application in the analysis and determination of estrogens in environmental water samples.

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JOURNAL OF CHROMATOGRAPHIC SCIENCE · 2021 ·Vol. 60 ·期 2 ·105-110 · IF 1.618

Development and Validation of a Sensitive GC–MS/MS Method for the Determination of Five Potential Genotoxic Impurities in Abiraterone Acetate

Zhong ZhenHua,Chen YuPing,Xia HongYing,Chen ZhenZhen,Cheng QiZhen

A sensitive and selective gas chromatography–tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The linearity was established for the concentration range of 30–480 ng/mL (2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate) and 90–1440 ng/mL (chloromethane). The correlation coefficient of each PGIs was >0.995. The extraction recoveries ranged from 90.49 to 106.79% for the five PGIs. The quantitation limit, detection limit, accuracy, precision, repeatability and stability of the method demonstrated that the method was an adequate quality control tool for quantitation and identification of chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate at trace levels in drug substances and drug products.

CAS / MDL: 75-26-3 75-29-6 64-67-5
✓ 已验证 产品关联 DOI PubMed 高影响因子
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2021 · IF 4.952

Characterization of key off-odor compounds in thermal duck egg gels by GC-olfactometry-MS, odor activity values, and aroma recombination

Liuyang Ren,Jie Ma,Ying Lv,Qigen Tong,Huiyuan Guo

Characterization of volatile off-odor compounds in thermal duck egg gels was investigated by gas chromatography-olfactometry-mass spectrometry (GC-O-MS), odor activity values (OAVs) and aroma recombination. The results demonstrated that the off-odor of thermal duck egg mainly came from egg yolk (EY), and content of aldehydes was the highest in EY. Anaerobic treatment in nitrogen contributed to decreased off-odor sensory scores and volatile components of the heated egg gels. Aerobic EY gels (treated in air) were determined to contain eight volatile compounds with OAVs greater than 1, such as hexanal, nonanal, benzaldehyde, ( E )-2-octenal, ( E )-2-nonenal, ( E, E )-2,4-decadienal, 1-octen-3-ol and 2-pentylfuran. However, three key volatile components (nonanal, benzaldehyde and ( E )-2-nonenal) with OAVs greater than 1 were found in anaerobic EY gels. Moreover, on the basis of results of recombination and omission experiments, hexanal, ( E )-2-octenal, ( E, E )-2,4-decadienal, 1-octen-3-ol and 2-pentylfuran were identified as key off-odor components in thermal EY gels. Sensory evaluation of the recombination model with five aroma compounds scored 4.38 out of 5 points. The major aroma profile of the off-flavor from egg EY gels included strong fatty, nutty, and mushroom aromas.

CAS / MDL: 25013-16-5
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ENVIRONMENTAL POLLUTION · 2020 · IF 6.793

Separation and identification of microplastics in marine organisms by TGA-FTIR-GC/MS: A case study of mussels from coastal China

Yi Liu,Ruojia Li,Jianping Yu,Fengli Ni,Yingfei Sheng,Austin Scircle,James V. Cizdziel,Ying Zhou

Microplastics are ubiquitous in the marine environment but characterizing them in marine organisms is challenging. Herein we describe a method to detect, identify, and quantify microplastics in marine mussels ( Mytilus edulis ) using thermal gravimetric analysis – Fourier Transform infrared spectroscopy – gas chromatography mass spectrometry (TGA-FTIR-GC/MS) after extracting and isolating the microplastics using chemical digestion, density separation, and filtration. Combining the three instrumental techniques adds discriminatory power as temperature profiles, chromatograms, and vibrational and mass spectra differ among common plastics. First, we tested several digestion schemes after spiking the mussels with plastics commonly found in the marine environment, including polyethylene (PE), polystyrene (PS), polypropylene (PP) and polyvinyl chloride (PVC). KOH (10%, w/v) was the most suitable reagent, providing good recoveries (>97%) without degrading the microplastics. We show that the technique TGA-FTIR-GC/MS can be optimized to readily determine both the type (polymer) and amount (mass) of microplastics in the sample. Applied to 100 mussels from each of six locations along the coast of China, we found an average of 0.58 mg of plastic per kg of tissue (range 0.16–1.71 mg/kg), with PE being the most abundant type of plastic measured. Among the coastal cities, mussels from Dalian had the highest microplastic content. Overall, we demonstrate that the method is a powerful technique to quantify masses of microplastics in marine mussels, a species commonly used as a bioindicator of pollution, and may be applied to other biota as well.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD RESEARCH INTERNATIONAL · 2021 · IF 6.475

Characterization of aroma and bacteria profiles of Sichuan industrial paocai by HS-SPME-GC-O-MS and 16S rRNA amplicon sequencing

Yajiao Zhao,Wenli Wei,Li Tang,Dongdong Wang,Yan Wang,Zhengyun Wu,Wenxue Zhang

Sichuan industrial paocai and traditional home-made paocai have different aroma profiles due to different manufacturing techniques, but detailed information about the aroma profiles and aroma-producing microorganism of Sichuan industrial paocai remain largely elusive. For this reason, we established and validated an external standard method of headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC–MS) combined with gas chromatography–olfactometry (GC-O) for identification and accurate quantitation of aroma-active compounds in Sichuan industrial paocai. This method was combined with 16S rRNA amplicon sequencing to comprehensively analyze the aroma and bacteria profiles of Sichuan industrial paocai. A total of 121 volatile compounds were identified, among which 36 odorants were identified as aroma-active compounds with aroma intensities (AIs) ranging from 0.67 to 5.00 by GC-O. The types of aroma-active compounds in Sichuan industrial paocai were variety-specific to some extent, but the aroma-active compounds shared by different varieties of Sichuan industrial paocai (i.e., skeleton aroma-active compounds) were phenylethyl alcohol, acetic acid, butanoic acid, 2-methylbutanoic acid, ethyl hexanoate, 4-ethylphenol and 4-ethylguaiacol. Moreover, 17 key aroma-active compounds of AI > 1 in radish paocai were quantitated by external standard method, and their odor activity values (OAVs) were calculated based on the odor thresholds. Further, 12 aroma-active compounds with OAV ≥ 1 in one of the radish paocai were selected to construct the recombination model, which revealed good agreement with the original sample. Furthermore, Lactobacillus, Pediococcus, Pseudomonas and Sphingomonas were the dominant bacteria in Sichuan industrial paocai. Correlation analysis between 16 dominant bacteria and 36 aroma-active compounds showed that Pediococcus, Arcobacter and Lactobacillus could be the core aroma-producing bacteria of Sichuan industrial paocai.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2021 · IF 7.514

Analysis of flavor formation during production of Dezhou braised chicken using headspace-gas chromatography-ion mobility spec-trometry (HS-GC-IMS)

Wensheng Yao,Yingxuan Cai,Dengyong Liu,Yu Chen,Jianrong Li,Mingcheng Zhang,Na Chen,Hao Zhang

In order to help the poultry industry to generate higher quality products, the headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) technique was used to identify volatile substances formed during the processing of Dezhou braised chicken (DBC). A total of 37 volatile substances including aldehydes, alcohols, ketones, esters, terpenoids, furans and pyrazines were identified during DBC processing across seven sampling stages. The analyses identified 2-ethylhexanol as a key flavor chemical within the chicken carcasses, and found that ethyl acetate, 1-hexanol, 4-methyl-2-pentanone and 1-pentanol were mainly produced during the deep-frying stage of processing. Stewing with herbs and spices was found to be an important stage in the flavor impartation process. 2-Butanone, n -nonanal, heptanal and ethanol were positively related to processing stage 3, whereas processing stage 4 was characterized by ethyl propanoate, benzaldehyde, butyl acetate, 2-pentyl furan and 2-heptanone. The processing stages 5, 6 and 7 were not significantly different (P > 0.05) from each other.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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CARBOHYDRATE POLYMERS · 2019 · IF 6.044

Study on cellulose degradation induced by hydroxyl radical with cellobiose as a model using GC–MS, ReaxFF simulation and DFT computation

Chunfu Shao,Qiang Shao,Xiaoyi Wang,Jun Ling,Xiao Guo,Yulin Ning,Yujie Dai,Shiru Jia,Yuanyuan Qiao,Changwen Li,Kai Zhao

The OH induced cellulose degradation was examined by analyzing the reaction products of Fenton’s regents with cellobiose. Many degradation products including C2-C5 compounds such as oxaldehyde, malonaldehyde and 2-hydroxysuccinaldehyde were detected by GC MS analysis. Four reaction pathways for the formation of some degradation products were obtained from ReaxFF kinetics simulation and validated by the DFT quantum chemistry calculation at B3LYP/6-31+g(d,p) level. It was found that the H-abstraction from OH of the glucose unit by OH can cause saccharide ring open and breakage of the glycosidic bond. Pathways 1–4 showed that the glucose unit can react with OH consecutively to produce small molecular products with carbon atoms less than 6. This study indicated that ReaxFF reaction kinetics is a powerful tool for the exploration of the degradation mechanism of cellulose induced by OH at room temperature, which correlated well with the experimental results and was validated by DFT calculation.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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NEW JOURNAL OF CHEMISTRY · 2019 ·Vol. 43 ·期 9 ·3946-3955 · IF 3.069

Single particle ICP-MS and GC-MS provide a new insight into the formation mechanisms during the green synthesis of AgNPs

Huiling Zhang,Yuxiong Huang,Jianqiang Gu,Arturo Keller,Yuwei Qin,Yue Bian,Kun Tang,Xiaolei Qu,Rong Ji,Lijuan Zhao

Green synthesis of metallic nanoparticles (NPs) using plant extracts has received considerable attention due to its environmentally and economically friendly nature. Various metabolites in plants such as amino acids, organic acids, sugars and phenolic compounds have been speculated to be responsible for the synthesis of metallic NPs in previous studies. However, to date, there has been a lack of direct evidence linking specific metabolites to the reduction of metal ions to form metallic NPs. Here, AgNPs are synthesized using cucumber leaf extract and characterized by UV-visible spectroscopy, dynamic light scattering (DLS) and transmission electron spectroscopy (TEM). Single particle inductively coupled plasma mass spectrometry (sp-ICP-MS) was used to investigate the size of newly synthesized NPs as well as the kinetics of particle formation. Gas chromatography–mass spectrometry (GC-MS) based metabolomics identified and quantified 245 metabolites in cucumber leaf extracts. By comparing the concentrations of metabolites before and after the reaction, the metabolites responsible for the synthesis were screened out. Reducing sugars (cellobiose, ribulose-5-phosphate, melibiose, 2-deoxy-D-glucose, tagatose, fructose, ribose, 3,6-anhydro-D-galactose) were markedly decreased after the reaction, indicating that reducing sugars are involved in the biosynthesis process and possibly function as reducing agents. The key thermodynamic data of the reaction between Ag+ and reducing sugars were obtained by using isothermal titration calorimetry (ITC), which further confirmed the interaction between Ag+ and metabolites. This study provides a deep insight into the reaction process and mechanism of green synthesized AgNPs.

CAS / MDL: 1336-21-6
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JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS · 2019 · IF 3.47

Diverse impact of α-Fe2O3 with nano/micro-sized shapes on the catalytic fast pyrolysis of pinewood: Py-GC/MS study

Adel Baimoldina,Konstantinos Papadikis,Elena Yu. Konysheva

The feasibility of α-Fe 2 O 3 catalyst addition in the in-situ catalytic fast pyrolysis of Pinewood was considered with the focus on the variation in its shape: nano-sized non-ideal spheres, nanotubes, hollow nano/microtubes, and octadecahedral crystals. Nano-sized spheres strongly promoted the formation of acetaldehyde, something that was also observed for the octadecahedral crystals. The formation of acids was primarily facilitated through the addition of nanotube catalysts and octadecahedral crystals. Newly formed alicyclic ketonic compounds were promoted through the addition of nano-sized spheres, hollow nano/microtubes, and octadecahedral crystals. The latter two catalysts also showed a moderate selectivity in the formation of furfural. All applied catalysts showed loss of activity, though at different degrees, on the formation of lignin derived phenolic compounds, which can be primarily attributed to favoring the formation of char with simultaneous release of CO 2 . All used α-Fe 2 O 3 catalysts with different shapes maintained their original morphology after the rapid heating with the rate of 20 K/ms followed by catalytic fast pyrolysis at 500 °C, indicating that nanomaterials with targeted dimensions can be applied as catalysts in the catalytic fast pyrolysis of biomass to enhance conversion of undesired oxygenated compounds to higher quality bio-oil and valuable chemicals.

CAS / MDL: 1309-37-1 7681-49-4
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CHROMATOGRAPHIA · 2013 ·Vol. 76 ·期 11 ·671-678 · IF 1.437

Ultra-Preconcentration and Determination of Multiple Pesticide Residues in Water Samples Using Ultrasound-Assisted Dispersive Liquid–Liquid Microextraction and GC-FID

Cui Shumin,Chen Qianxia,Wang Weiping,Miao Jigen,Wang Aijun,Chen Jianrong

In this study, a simple and efficient method has been developed to analyze pesticides in water samples using ultrasonic-assisted dispersive liquid–liquid microextraction (UA-DLLME) combined with gas chromatography-flame ionization detection (GC-FID). Several parameters, including type and volume of extractant and dispersant, extraction time, and amount of salt on extraction performance, were optimized in detail. A mixture of acetonitrile (1.0 mL, dispersant) and carbon tetrachloride (15 μL, extractant) was used for extraction. Under optimal conditions, enrichment factors were obtained between 315 and 1153. The linearity of the method ranged from 1 to 100 μg L −1 with correlation coefficients ≥0.9990. Limits of detection (S/N = 3) ranged between 0.09 and 0.57 μg L −1 , depending on the compounds. Relative standard deviations were <8.0 % ( n  = 5) for both intra- and inter-day analyses. The proposed method was successfully applied for the preconcentration and determination of pesticides in water samples (river water, tap water, and lake water) with recoveries that varied from 90.5 to 107.7 %.

✓ 已验证 产品关联 DOI 高影响因子
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CHINESE CHEMICAL LETTERS · 2015 · IF 1.587

Magnetic nanoparticles used in headspace extraction coupled with DSI-GC-IT/MS for analysis of VOCs in dry Traditional Chinese Medicine

Jing Nie,Yuan-Jie Teng,Zu-Guang Li,Wen-Han Liu,Maw-Rong Lee

A novel magnetic method using polystyrene modified magnetic nanoparticles to perform thermo-headspace extraction was successfully developed for extraction and preconcentration of volatile organic components in dry Traditional Chinese Medicine (TCM) based on gas chromatography-ion trap/mass spectrometry with a ChromatoProbe direct sample introduction device. The dried fruit of Amomum testaceum Ridl. was used as the object TCM. The optimum parameters of headspace magnetic solid-phase extraction were investigated, in which desorption solvent ethyl acetate played a key role in this method, and the headspace extraction temperature of 90   °C and the headspace extraction time of 15   min finally decided. Headspace solid-phase microextraction method was also used to analyze volatile compounds in the TCM to compare with the proposed method. The results show that 60 components were identified totally by two methods; most of the low boiling point chemical compounds are isolated by this new method. In this work, an environmental-friendly and cheap analytical method was established, and a new approach to analyze volatile compounds in dry Traditional Chinese Medicine was also provided.

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