Analytical Methods
·
2023
·Vol. 15
·期 6
·849-858
·
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 CHEMISTRY
·
2022
·
IF 9.231
Long Xu,Hao Cheng,Marco Müller,Andrew J. Sinclair,Weifei Wang,Xuhua Guo,Walter Vetter,Yonghua Wang
Furan fatty acids (FuFAs) have been recognized as beneficial food ingredients to human health. Herein, a targeted quantitation approach by gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC-TQ/MS) was developed for the identification of FuFAs in common marine and other edible oils in multiple reaction monitoring (MRM) mode without any isolation and enrichment. The limit-of-quantitation (LOQ, 0.6 pg) was determined under the optimized parameters in MRM mode. Identification of FuFAs in common edible oils demonstrated that marine fish oils were concentrated sources of 9-(3-methyl-5-pentylfuran-2-yl)nonanoic acid (9M5), 11-(3,4-dimethyl-5-propylfuran-2-yl)undecanoic acid (11D3) and 11-(3,4-dimethyl-5-pentylfuran-2-yl)undecanoic acid (11D5). However, FuFAs were not identified in common plant oils. Additionally, 11D5 was identified in the lipids of Schizochytrium limacinum at a comparable level with that in marine fish oil. We believe that this protocol could facilitate the qualitative and quantitative analysis of FuFAs in food and biological samples.
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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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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 14
·3325-3335
·
IF 3.307
Liu Yue,Lu Shan,Zhao Liang,Dong Xin,Zhu Zhenyu,Jin Yongsheng,Chen Haisheng,Lu Feng,Hong Zhanying,Chai Yifeng
Studies have documented the potential antitumor activities of glaucocalyxin A (GLA), an ent-kaurene diterpenoid isolated from Rabdosia japonica . However, the metabolic mechanism underlying the antitumor activity of GLA remains largely unknown. The effects of GLA on the metabolome of human liver cancer cells using GC/MS- and LC/MS-based metabolic profiling have been investigated. An untargeted metabolomics approach in conjunction with orthogonal projection to latent structures–discriminant analysis (OPLS-DA) has been developed to characterize the metabolic modifications induced by GLA treatment in human hepatoma cell line SMMC7721. Results demonstrated that cells cultured in the presence or absence of GLA displayed different metabolic profiles: the treatment induced an increased purine metabolism, pyrimidine metabolism, and sphingolipid metabolism and a decreased amino acid metabolism. At the same time, GLA treatment induced cell apoptosis and cell cycle arrested at G2/M phase in a dose-dependent manner. In addition, two representative apoptosis-inducing cytotoxic agents were selected as positive control drugs to validate the reasonableness and accuracy of our metabolomic investigation on GLA. The study displayed a systemic metabolic alteration induced by GLA treatment, showing the impaired physiological activity of SMMC7721 cells, which also indicated anti-proliferative and apoptotic effects of GLA. In the meantime, GC/MS- and LC/MS-based metabolomics applied to cell culture enhanced our current understanding of the metabolic response to GLA treatment and its mechanism; such an approach could be transferred to study the mechanism of other anticancer drugs.
A systemic metabolic alteration induced by glaucocalyxin A (GLA) treatment of SMMC-7721 cells
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INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2023
·Vol. 24
·期 19
·14988
·
IF 5.6
Yuan Zhong,Zhilong Jia,Hailong Zhou,Dan Zhang,Guichen Li,Jihua Yu
The ultrasonic cell disruption method was used to efficiently extract isothiocyanates and other volatile compounds from radish microgreens. A total of 51 volatiles were identified and quantified by headspace solid-phase micro-extraction and gas chromatography–mass spectrometry (HS-SPME/GC–MS) in four radish microgreen cultivars, mainly including alcohols, aldehydes, isothiocyanates, sulfides, ketones, esters, terpenes, and hydrocarbons. The correlation between cultivars and volatile compounds was determined by chemometrics analysis, including principal component analysis (PCA) and hierarchical clustering heat maps. The aroma profiles were distinguished based on the odor activity value (OAV), odor contribution rate (OCR), and radar fingerprint chart (RFC) of volatile compounds. This study not only revealed the different flavor characteristics in four cultivars but also established a theoretical basis for the genetic improvement of radish microgreen flavors.Keywords:flavor;volatile compounds;radish microgreens;ultrasonic cell disruption;GC–MS
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BIOLOGICAL TRACE ELEMENT RESEARCH
·
2023
·
IF 3.9
Peng Hui- xin,Chai Fu,Chen Ke-heng,Huang Yan-xin,Wei Guang-ji,Yuan Huixiong,Pang Yan-fang,Luo Shi-hua,Wang Chun-fang,Chen Wen-cheng
Aluminum chloride is an inorganic polymeric coagulant commonly found in daily life and various materials. Although male reproductive toxicity has been associated with AlCl 3 exposure, the underlying mechanism remains unclear. This study aimed to examine the impact of AlCl 3 exposure on mitophagy and mitochondrial apoptosis in testicular tissue and mouse spermatocytes. Reactive oxygen species (ROS) and ATP levels were measured in GC-2spd after AlCl 3 exposure using a multifunctional enzyme labeler. The changes in mitochondrial membrane potential (MMP) and TUNEL were observed through confocal laser microscopy, and the expression of proteins associated with mitophagy and apoptosis was analyzed using Western blot. Our results demonstrated that AlCl 3 exposure disrupted mitophagy and increased apoptosis-related protein expression in testicular tissues. In the in vitro experiments, AlCl 3 exposure induced ROS production, suppressed cell viability and ATP production, and caused a decrease in MMP, leading to mitophagy and cell apoptosis in GC-2spd cells. Intervention with N-acetylcysteine (NAC) reduced ROS production and partially restored mitochondrial function, thereby reversing the resulting mitophagy and cell apoptosis. Our findings provide evidence that ROS-mediated mitophagy and cell apoptosis play a crucial role in the toxicity of AlCl 3 exposure in GC-2spd. These results contribute to the understanding of male reproductive toxicity caused by AlCl 3 exposure and offer a foundation for future research in this area.
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JOURNAL OF FOOD SCIENCE
·
2021
·Vol. 86
·期 3
·813-823
·
IF 3.167
Wei Chen,Dandan Qi,Wenwen Wang,Aiqing Miao,Chengying Ma
The study was aim to investigate the effects of grafting on volatile compounds and sensory quality of black tea. Seven groups of black tea were prepared from one nongrafted tea tree “Yinghong9 (YJ)” and six grafted tea trees by grafting scion of “YingHong9” on different rootstocks. Sensory analysis indicated marked/slight variations among seven samples, among which, the one grafting on HuangZhiXiangDanCong (HZX) stood out with floral and fruity aroma. The result of chemometrics analysis suggested various effects on compounds caused by different rootstocks. A total of 38 differential compounds were identified, showing mainly quantitative variations, with 36 being identified in all samples. The significant higher contents of volatiles, such as geraniol, phenylethyl alcohol, ( E )-nerolidol, decanal, and linalool oxides, in HZX compared with YJ were observed, which explained why floral and fruity aroma stood out among the whole aroma profile of HZX. Both results of sensory and instrumental analysis suggested certain correlation between compound variations and aroma characteristics. Moreover, different rootstocks influenced the aroma quality in different ways. Practical Application In conclusion, the study illuminates the various effects of grafting on the volatile compounds and aroma quality, which enlightens the possibility of changing aroma quality of black tea by grafting scions on different rootstocks. And thus, it can help guide the practical production when cultivating new varieties.
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JOURNAL OF ALLOYS AND COMPOUNDS
·
2021
·
IF 5.316
Jiangshan Gao,Huanhuan Wang,Yang Zhou,Zhiming Liu,Yan He
The combination of magnetic nanoparticles and transition metal oxides has attracted much attention in microwave absorption applications. Herein, the MnO 2 /Mn 3 O 4 @Ni-Co/graphite carbon (GC) nanocubes with porous structure and ultrathin nanosheets was constructed by self-template strategy and in-situ synthesis. The composites not only synergize the magnetic loss of magnetic Ni-Co nanoparticles with the dielectric losses of GC and MnO 2 /Mn 3 O 4 , but also enhance the multiple interface polarization and improve impedance matching. As a result, the MnO 2 /Mn 3 O 4 @Ni-Co/GC nanocubes present outstanding electromagnetic wave (EMW) absorption performances, in which a RL min of −26 dB at 6.4 GHz with a thickness of 4 mm and an effective absorption bandwidth covering from 5.3 GHz to 6.4 GHz are achieved. Meanwhile, the widest effective absorption bandwidth with the value of 3.7 GHz can be achieved at a matching thickness of 2.0 mm. More importantly, this work provides a new strategy for the synthesis of EMW absorbing materials.
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ANALYTICAL BIOCHEMISTRY
·
2021
·
IF 3.365
Xin Liu,Jihong Fu,Lili Wang,Caijuan Wang
A novel microwave-assisted (MA) headspace solid-phase extraction (HS-SPE) based on polydimethylsiloxane (PDMS)/ZIF-8@GO sponge was developed for the simultaneous extraction and determination of essential oil constituents in lavender. The PDMS/ZIF-8@GO sponge with a high surface area and excellent adsorption capacity was successfully applied in the HS-SPE process. Microwave-assisted coupled with PDMS/ZIF-8@GO sponge headspace solid-phase extraction followed by GC-MS was proposed. Different experimental parameters were investigated. The optimal conditions were found to be as follows: 2:1 as the quality ratio of ZIF-8 to GO , ZIF-8@GO dosage of 30 mg, microwave power of 600 W, extraction time of 10 min and desorption solvent of n -hexane. This method was successfully applied to the analysis of 11 samples of lavender in different varieties. A total of 52 compounds were identified by the proposed method. A good linearity was observed from 14 to 800 ng with a correlation coefficient (R 2 ) value of >0.99. Multivariate statistical analysis was used to establish the relationship between the varieties and the volatile components for further discriminant analysis. These results demonstrated that the MA-PDMS/ZIF-8@GO is an efficient, sensitive and small sample consumption method for the determination of the essential oil in dried plant materials.
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BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 12
·e5209
·
IF 1.902
Yunheng Yao,Longlv Bai,Haifeng Tian,Xinzi Wu,Nianjie Zhang,Lunpeng Wu,Yifan Jia,Xiuli Ren
In this study, a new fluorinated methacrylamide (MACF) was synthesized and evaluated as an adsorbent in the dispersive solid-phase extraction for the effective determination and extraction of 20 organophosphorus pesticides (OPPs) from ginseng samples using the QuEChERS (quick, easy, cheap, effective, rugged, safe) method coupled with GC–MS/MS. The properties of MACF were characterized using Fourier-transform infrared spectroscopy, elemental analysis, and high-resolution 19 F NMR. MACF, chitosan, primary and secondary amine, octadecylsilane, graphitized carbon black, Z-Sep, Z-Sep + , and EMR-Lipid were compared in terms of extraction efficiency. The best results were obtained when MACF was used. Matrix-matched calibration was employed for quantification. All the OPPs exhibited good linearity ( r 2 > 0.9969) with the concentration at their respective concentration ranges. The limits of detection were 1.5–3.0 μg/kg, and the limits of quantification were 5.0–10.0 μg/kg. The trueness of the 20 pesticides at four spiked levels ranged from 86.1 to 111.1%, and the relative standard deviation was less than 11.3%. The modified QuEChERS method using MACF as the adsorbent was sensitive, reliable, and cost-effective and could be used for the determination of 20 OPP residues in ginseng.
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Biomass Conversion and Biorefinery
·
2021
·Vol. 13
·期 13
·11789-11802
·
IF 4.987
Zhang Liqiang,Liu Jiaojiao,Zhang Zexia,Yang Zhengda,Wang Xinwei,Li Dawei,Lin Riyi
Two-step pyrolysis (TSP) of cellulose, hemicellulose, and lignin; the three-component cross-coupling samples; and the acid-washed walnut shell (AWS) were carried out by a pyrolysis–gas chromatography/mass spectrometry (Py-GC/MS) to investigate the effects of components and their proportions on the TSP of biomass. The results showed that different components dominated the formation of different products. Cellulose generated more furans and carbohydrates in both the first (S1) and second steps (S2). Hemicellulose achieved higher selectivity of ketones, acids, and alcohols in S1, and higher selectivity of hydrocarbons in S2. Lignin mainly produced phenols in S1, and hydrocarbons and phenols in S2. The increase of holocellulose (hemicellulose and cellulose) improved the contents of aldehydes, ketones, furans, acids, and alcohols but reduced the content of phenols in S1. In S2, more holocellulose increased the contents of aldehydes, ketones, and acids, but decreased the contents of phenols, hydrocarbons, and alcohols. The generation of carbohydrates was strongly inhibited in S1 by hemicellulose and lignin. More cellulose improved the contents of aldehydes, acids, and furans in S1, and increased the content of ketones but reduced the content of acids in S2. Hemicellulose facilitated the generation of hydrocarbons, but inhabited the produce of carbohydrates in S2. The small amount of the low-content components (protein, alkali and alkaline earth metals, etc.) and the connection structure of the components resulted in the significant difference in the pyrolysis reactions and product distribution of AWS and the mixed sample with corresponding component proportion. Therefore, more influence factors, such as the low-content components, the connection structure of the components, and different pyrolysis conditions, should be considered in the near future to investigate the interactions on the two or more components in TSP.
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