FOOD CHEMISTRY
·
2023
·
IF 8.8
Jing-Jing Zhang,Yan Gao,Mei-Ling Zhao,Xiao Xu,Bo-Nan Xi,Li-Ke Lin,Jing-Yi Zheng,Bang Chen,Yu Shu,Cong Li,Yehua Shen
Authentication of walnut oil (WO) is challenging due to the adulteration of high-linoleic acid vegetable oils (HLOs) with similar fatty acid composition. To allow the discrimination of WO adulteration, a rapid, sensitive and stable scanning method based on supercritical fluid chromatography quadrupole time-of-flight mass spectrometry (SFC-QTOF-MS) was established to profile 59 potential triacylglycerol (TAGs) in HLOs samples within 10 min. Limit of quantitation of the proposed method is 0.002 µg mL −1 and the relative standard deviations range from 0.7% to 12.0%. TAGs profiles of WO samples from various varieties, geography origins, ripeness, and processing methods were used to construct orthogonal partial least squares-discriminant analysis (OPLS-DA) and OPLS models that were highly accurate in both qualitative and quantitative prediction at adulteration levels as low as 5% (w/w). This study advances the TAGs analysis to characterize vegetable oils and holds promise as an efficient method for oil authentication.
研究领域:
食品科学
·
分析化学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Yang Huang,Ying Feng,Guangyun Tang,Minyi Li,Tingting Zhang,Marianne Fillet,Jacques Crommen,Zhengjin Jiang
Flavonoids from plants always show a wide range of biological activities. In the present study, a rapid and highly efficient supercritical fluid chromatography (SFC) method was developed for the separation of 12 flavonoids. After careful optimization, the 12 flavonoids were baseline separated on a ZORBAX RX-SIL column using gradient elution. A 0.1% phosphoric acid solution in methanol was found to be the most suitable polar mobile phase component for the separation of flavonoids. From the viewpoint of retention and resolution, a backpressure of 200 bar and a temperature of 40 °C were shown to give the best results. Compared with a previously developed reverse phase liquid chromatography method, the SFC method could provide flavonoid separations that were about three times faster, while maintaining good peak shape and comparable peak efficiency. This SFC method was validated and applied to the analysis of five flavonoids (kaempferol, luteolin, quercetin, luteoloside, buddleoside) present in Chrysanthemum morifolium Ramat. from different cultivars (Chuju, Gongju, Hangju, Boju). The results indicated a good repeatability and sensitivity for the quantification of the five analytes with RSDs for overall precision lower than 3%. The limits of detection ranged from 0.73 to 2.34 μg/mL, while the limits of quantification were between 2.19 and 5.86 μg/mL. The method showed that SFC could be employed as a useful tool for the quality assessment of Traditional Chinese medicines (TCMs) containing flavonoids as active components.
研究领域:
分析化学
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生药学
·
药物分析
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PubMed
高影响因子
CHROMATOGRAPHIA
·
2017
·Vol. 80
·期 8
·1179-1188
·
IF 1.402
Li Ben,Guo Wei,Chi Haijun,Kimura Masaru,Ramsey Edward D.
A high-pressure photochemical reaction cell operated with a magnetic stir drive has been directly interfaced on-line with either SFC or HPLC. The interface consisted of an oven housing a recirculation pump directly connected to a sample injection valve. The inlet of the recirculation pump and the outlet from the sample injection valve were connected to the stirred reaction cell such that a return flow circuit was established. With this arrangement, a continuous flow of fresh supercritical fluid photochemical reaction mixture was maintained through the sample injection valve. This enabled samples of reaction mixture to be conveniently analyzed at regular intervals to monitor reaction progress using either on-line SFC or HPLC. The photoreduction of benzophenone in the presence of propan-2-ol to produce 1,1,2,2-tetraphenylethane-1,2-diol and 2-methyl-1,1-diphenylpropan-1,2-diol was studied. For this reaction, on-line SFC provided significantly better performance than on-line HPLC and was therefore used to monitor overall reaction progress and the different product yields. Quantitative results for this study demonstrate that highly efficient photochemical reactions proceeded in supercritical fluid carbon dioxide at 13 and 20 MPa.
研究领域:
化工工程
·
分析化学
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光化学
·
超临界流体技术
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DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Jinlei Yang,Tianyi Liao,Pingping Zhang,Runsong Cheng,Jing Wang,Siyuan Pan,Murong Du,Boya Zhao,Weiliang Liu,Liying Yan,Sichun Zhang,Xinrong Zhang
Lipid regulation and remodeling are pivotal in follicle development and oocyte maturation. Performing lipidome analysis on single oocytes is essential for optimizing assisted reproductive techniques and improving pregnancy outcomes. Conventional organic solvent extraction faces challenges in single-cell analysis, including excessive sample dilution and time-consuming processing. In this study, we developed an on-valve microflow supercritical fluid extraction and chromatography–mass spectrometry (μSFE-SFC-MS) method. Lipids in intact single oocytes are extracted online by supercritical carbon dioxide fluid, separated by a C18 capillary column, ionized, and annotated. Notably, this method significantly reduces sample pretreatment and chromatographic separation time to just 15 min per sample, compared to about 2 h of the conventional method. We analyzed of 276 lipid species from a single oocyte. Lipidomic differences in oocyte maturation stages clarify distinct metabolic remodeling of phospholipids into sphingomyelins and glycerides. The differential analysis suggests that several lipid species can be used as criteria for determining oocyte maturation at the single-cell level. The present work offers a fast and high-coverage lipidomic analysis for single oocytes, also providing a workflow for other single-cell and trace samples.
研究领域:
分析化学
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脂质组学
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生殖生物学
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质谱分析
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色谱分析
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代谢组学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Qing Fu,Wenwen Dong,Dandan Ge,Yanxiong Ke,Yu Jin
The development of an approach based on simultaneous supercritical fluid extraction-sample cleanup, followed by supercritical fluid chromatography/tandem mass spectrometry (SFE-SFC-MS/MS) was as a tool for the extraction, separation and characterization of indole alkaloids of Uncaria rhynchophylla . A two-step SFE method was designed. A mixture of the U. rhynchophylla sample and an adsorbent named C18SCX with the ratio of 1:1 (w/w) was placed into an extraction cell. The extraction temperature was 40 °C and the pressure was 25 Mpa. In the first step, 10 % EtOH as the co-solvent was used to extract for 60 min, which was considered as a cleanup process to remove non-alkaloid components. In the second step, 0.1 % DEA was added to 10 % EtOH and it extracted for 60 min to obtain the desired extract. By introducing an additional adsorbent, the specificity of SFE towards alkaloids was greatly improved. An SFC-MS/MS method was then utilized for analysis of the SFE extract. Using 2-EP as stationary phase with the gradient elution of 0–10 min, 5–25 % EtOH (+0.05 % DEA) in CO 2 , column temperature 40 °C, and back pressure 13.8 Mpa, 10 peaks were separated within 8 min. Further MS/MS analysis confirmed that nine of the 10 peaks in the SFE extract were indole alkaloids. This study developed a supercritical fluid-based method specifically towards extraction and analysis of alkaloids, which is helpful to the study of alkaline compounds in complex samples.
研究领域:
植物化学
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分析化学
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药学
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PubMed
高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 9
·1257-1267
·
IF 1.401
Guo Wei,Li Ben,Chi Haijun,Ramsey Edward D.
Abstract The operation of a SFC–MS system has been improved. The SFC–MS interface uses a post-column make-up flow of liquid whose supply line to the SFC–MS interface mixing tee is equipped with an injection valve. Prior to analysis, this arrangement permits a stable flow of a dilute tune solution of analyte(s) for the exact amount of time required to optimize mass spectrometry tuning. Advantageously, with this arrangement tuning is performed in the presence of the exact split flow and same composition of SFC mobile phase and make-up liquid to be used for subsequent SFC–MS operation. The SFC–MS interface was constructed to provide a pre-back pressure regulator split flow to the mass spectrometer using a linear restrictor. Two different linear restrictors constructed from either 50 µm i.d. PEEK tubing or 25 µm i.d. fused silica tubing were evaluated. For best electrospray performance, each restrictor required a different post-column make-up flow rate. The use of either restrictor retained a high degree of chromatographic fidelity for the SFC separation of six pharmaceutical compounds using a cyanopropyl column with a mobile phase of supercritical fluid carbon dioxide modified with methanol and aqueous ammonia solution. Each restrictor provided a different level of SFC–MS performance for each of the six pharmaceutical compounds tested. Based upon overall performance, a linear fused silica restrictor was selected to develop a chromatographic separation using on-line SFC–MS for three structurally very similar monensin sodium salt analogues that are not directly amenable to off-line SFC using UV/Vis detection. Graphical abstract
研究领域:
分析化学
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质谱分析
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色谱技术
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高影响因子
JOURNAL OF THE AMERICAN OIL CHEMISTS SOCIETY
·
2016
·Vol. 93
·期 9
·1173-1182
·
IF 1.505
Qi Wei,Yue Wei,Haiwen Wu,Xiuyan Yang,Huangli Chen,Huaxin Zhang
The supercritical CO 2 fluid extraction process was used to obtain seed oils. The compositional analyses of the seed oils of Amorpha fruticosa L., Caragana microphylla Lam and Elaeagnus angustifolia L. were performed by GC–MS, from which 18–22 fatty acid compositions were identified, and their main components were linoleic acid (49.10–66.39 %) and oleic acid (11.95–41.10 %). The seed oils were rich in unsaturated fatty acids, which accounted for 79.75–91.19 %. The in vitro anti-oxidant activities of the seed oils were measured by the DPPH, ABTS and phosphomolybdenum complex assays. The IC 50 s of the seed oils were 6.5110–12.6599 mg/mL tested by DPPH assay, and the IC 50 s were in the range of 0.6872–1.9310 mg/mL tested by ABTS assay. The anti-oxidant activities of seed oils decreased in the order of A. fruticosa > C. microphylla > E. angustifolia (A) > E. angustifolia (D). In vitro antimicrobial activities of seed oils against five bacteria were tested by microdilution method. The MIC values of the oils against Bacillus subtilis , E. coli , S. aureus , P. solanacearum and B. thuringiensis were in the range of 26–36, 30–38, 58, 56–58 and 56–58 mg/mL, respectively, while the MBC values were in the range of 30–40, 34–42, 58, 56–58 and 58 mg/mL, respectively. In vitro antifungal properties of the seed oils against four plant pathogenic fungi were tested by the mycelial growth rate method. The EC 50 s of seed oils against V. mali , C. gloeosporioides , F. graminearum and B. cinerea were in the range of 17.51–19.25, 15.58–19.12, 8.00–17.12 and 18.76–19.14 mg/mL, respectively. The seed oils showed moderate anti-oxidant and antimicrobial activities.
研究领域:
植物学
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食品科学
·
药理学
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DOI
高影响因子
JOURNAL OF SUPERCRITICAL FLUIDS
·
2020
·
IF 3.744
Ben Li,Wei Guo,Edward D. Ramsey
A combined SFE-SFC system has enabled the simultaneous determination of the partition coefficient ( K ) values of three organic compounds distributed as mixtures between SF-CO 2 and water phases. The system used a single valve SFE-SFC recirculation interface. The compounds were: o -toluidine, o -cresol and indole prepared as mixtures in aqueous solutions at concentration levels applicable to industrial process waters and of relevance to potential groundwater contamination that may arise from geological carbon capture and storage facilities. Sets of three compound K values were simultaneously obtained at temperatures 313 K, 323 K, 333 K, and five pressures from 8.62 MPa to 22.41 MPa. At each temperature, the SFE vessel pressure was incremented in controlled SF-CO 2 pressure steps applied to a single stirred water sample to rapidly obtain complete series of individual K values. The instrumentation and method demonstrate considerable potential to achieve significant time savings to construct an expanded organic compound K database.
研究领域:
环境化学
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分析化学
·
超临界流体技术
·
绿色化学
·
污染科学
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DOI
高影响因子
JOURNAL OF SUPERCRITICAL FLUIDS
·
2023
·
IF 3.9
Wei Guo,Ben Li,Haijun Chi,Zhongliang Jiang,Liu Qing Wei,Edward D. Ramsey
Two flow selection interfaces have been developed for connecting single or linked reactors with on-line SFC equipped with UV/Vis diode-array (DAD) and mass spectrometer detectors coupled in series (SFC-DAD-MS). This process analytical technology system, enabled the study of reactions performed in supercritical fluid carbon dioxide (SF-CO 2 ). Each interface is designed to obtain on-line samples at different reaction progress points. Three single stage electrophilic annulation reactions performed in SF-CO 2 using aniline, indole and pyrrole as amine reactants to synthesize N-heterocyclic products within a stirred continuous flow reaction vessel containing montmorillonite K-10 catalyst were monitored. Also, both stages of a two step synthetic procedure conducted within two connected continuous flow reaction coil systems were monitored using on-line SFC-DAD-MS. The first step involved a Knoevenagel reaction in SF-CO 2 that provided a continuous feed to perform a second stage acetylation reaction. Use of on-line SFC-DAD-MS enabled early detection and characterization of unexpected by-products.
研究领域:
化学工程
·
分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Chunying Song,Gaowa Jin,Dongping Yu,Zhimou Guo,Xinmiao Liang
A novel silica stationary phase was designed and prepared through thiol-epoxy click chemistry for supercritical fluid chromatography (SFC). The developed stationary phase was characterized by elemental analysis, Fourier transform infrared spectrometry and solid-state 13 C/CP MAS NMR spectroscopy. In order to evaluate the chromatographic performance and retention mechanisms of the prepared column, a variety of alkaloids were used, including indoles, isoquinolines, pyrrolidines, piperidines, quinolizidines and organic amines. The stationary phase showed more symmetrical peak shapes and better performance for these compounds compared to the conventional SFC stationary phases. The investigations on the effects of pressure and temperature on retention provided information that the selectivity of the compounds can be improved by changing the density of the supercritical fluids. Moreover, it shows improved separation efficiency of three natural products with alkaloids as the main components at high sample loading. In conclusion, the developed stationary phase could offer flexible selectivity toward alkaloids and complex samples.
研究领域:
分析化学
·
色谱技术
·
超临界流体技术
·
有机化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Hao Zhang,Shu Wang,Shixiao Wei,Shangde Sun,Yanlan Bi,Mingfu Wang,Yueliang Zhao
A novel supercritical fluid chromatography coupled with tandem mass spectrometry (SFC-ESI-QqQ-MS/MS) method was developed for simultaneous quantification of malondialdehyde (MDA) and seven α,β-unsaturated aldehydes (α,β-UAs) in edible oils and oil-containing foods. Combining DNPH derivatization with one-step extraction, the method achieved exceptional performance: linearity (R 2 ≥ 0.9995), rapid analysis (16 min/sample), recoveries (85.84–106.71 %), and precision (RSD < 7.86 %), with LOD/LOQ at 0.05–0.60/0.15–1.80 μg/kg. This validated technique was subsequently applied to monitor the formation of MDA and α,β-UAs during the heating of eight edible oils, revealing concentration dependencies on fatty acid composition and heating duration. Furthermore, the levels of MDA and seven α,β-UAs in 29 oil-containing foods commonly consumed in China were determined using the developed method, with concentrations ranging from 2.65 to 326.79 μg/kg and 15.67–770.71 μg/kg, respectively. As the first SFC-based approach for comprehensive aldehyde profiling, this method enables precise monitoring of lipid oxidation pathways and supports quality control innovations in the food industry.
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高影响因子
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