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Journal of chromatography
Elesevier
Journal of chromatography

Elesevier

0021-9673

Journal of chromatography/Journal Journal of chromatographySCIISTPCCR
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    Designed 3D N-doped magnetic porous carbon spheres for sensitive monitoring of biogenic amine by simultaneous microwave-assisted derivatization and magnetic-solid phase extraction

    Xu, XuGao, JiaxinCao, DiLi, Xiang...
    10页
    查看更多>>摘要：In this paper, the novel 3D N-doped magnetic porous carbon spheres (3D N-MPCSs) was constructed via a simple template-free and self-doping method, followed by a direct carbonization of polymer with Fe3+ for simultaneous activation and magnetization. For the first time, the designed 3D N-MPCSs was used as multifunctional (for extraction and magnetic separation) adsorbents for microwave-assisted derivatization and magnetic solid phase extraction, which exhibited excellent extraction ability for its large surface area, mesoporous structure, spherical morphology, and incorporation of N/O heteroatoms. Moreover, when the microwave-assisted derivatization was combined with the magnetic solid phase extraction, the extraction, derivatization and concentration was completed simultaneously within 135 s. Furthermore, this method has a low detection limit (0.059-0.073 ng mL(-1)) and high enhancement factors (333 < EFs < 382) for trace biogenic amine (BAs). The recoveries were between 92.3 and 108.8% with relative standard devia-tions less than 5.9%. Overall, a simple, rapid, efficient and sensitive method for the analysis of BAs in food samples was developed, which provided the basis for routine detection of food safety. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Glutathione functionalized magnetic covalent organic frameworks with dual-hydrophilicity for highly efficient and selective enrichment of glycopeptides

    Song, JiayiYang, YiSu, PingLi, Meng...
    10页
    查看更多>>摘要：Glycoproteins can be used as biomarkers to detect many diseases. Reliable and efficient sample materials are essential to separate and enrich glycopeptides before detection and analysis. In this report, glutathione (GSH)-modified magnetic covalent organic framework (TpBD) composite Fe3O4@TpBD@Au@GSH was synthesized by a two-step, post-synthesis modification strategy. The native hydrophilic TpBD and the highly hydrophilic GSH furnished the composite with dual-hydrophilic performance that was superior to covalent organic framework-based materials reported previously. The composite material showed excellent performance in enriching glycopeptides from protein standards because of its superior hydrophilicity, with 21 and 36 glycopeptides enriched from horseradish peroxidase (HRP) and immunoglobulin G from human serum (IgG) tryptic digests, respectively. The prepared composite exhibited ultra-high sensitivity (0.1 fmol/mu L), excellent selectivity (HRP tryptic digest/bovine serum albumin (BSA) tryptic digest = 1:20 0 0) and macromolecular protein anti-interference ability (HRP tryptic digest/BSA = 1:20 0 0). Moreover, Fe3O4@TpBD@Au@GSH exhibited outstanding binding capacity (160 mg/g), excellent long-term storage capacity and good recycling ability (at least six times). Glycopeptide enrichment of biological samples by Fe3O4@TpBD@Au@GSH was successful, with 492 and 160 glycopeptides, corresponding to 134 and 64 glycoproteins, detected in 5 mu L human serum and human saliva samples, respectively. The results showed that Fe3O4@TpBD@Au@GSH provides more information to facilitate in-depth analysis of glycopeptides in biological samples and has broad potential in cancer monitoring and diagnosis. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    An ion mobility-enabled and high-efficiency hybrid scan approach in combination with ultra-high performance liquid chromatography enabling the comprehensive characterization of the multicomponents from Carthamus tinctorius

    Qian, Yue-xinZhao, Dong-xueWang, Hong-daSun, He...
    13页
    查看更多>>摘要：Liquid chromatography/mass spectrometry (LC/MS) is extensively applied for the untargeted/targeted analyses of the herbal components, utilizing data-dependent acquisition (DDA) or data-independent acquisition (DIA) to record the fragmentation information useful for the structural elucidation. A new trend recently has emerged by integrating DDA and DIA to render the hybrid scan, which, unfortunately, has rarely been reported. Herein, by using the Vion (TM) ion-mobility quadrupole time-of-flight mass spectrometer, a hybrid scan strategy (HDMSE-HDDDA) was presented and validated by the untargeted characterization of the multicomponents from Carthamus tinctorius (safflower), in combination with reversed phase ultra-high performance liquid chromatography (RP-UHPLC). Good chromatographic separation was achieved on an HSS T3 column within 26 min, while HDMSE-MS/MS was used to acquire the collision induced dissociation MS2 data in the negative mode. Automatic workflows (e.g., data correction, precursors/product ions matching, and peak annotation) were well established on UNIFI (TM) (incorporating an in-house library recording 261 known compounds) to process the obtained MS2 data. Compared with single DDA or DIA, the hybrid approach of HDMSE-HDDDA better balanced between the coverage and reliability, led to high-definition MS spectra, offered useful collision cross section (CCS) information, and showed satisfactory identification performance comparable to MSE. A total of 141 components (involving 41 quinochalcones, 66 flavanols/flavones, 11 flavanones, 6 organic acids, 1 polyacetylene, and 16 others) were characterized from safflower. Moreover, CCS prediction could assist isomers characterization, to some extent. Conclusively, this hybrid scan approach enables a dimension-enhanced MS data acquisition strategy providing the complementary structural information, which more suits the chemical characterization of complex samples. (C) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    High-throughput analysis of the steroid profile in placental cell cultures to evaluate endocrine disrupting effects of contaminant exposure

    Mestres, JuliaPerez-Albaladejo, ElisabetPorte, CintaPostigo, Cristina...
    8页
    查看更多>>摘要：Human placental JEG-3 cells conserve a high P450 aromatase activity and are therefore suitable to eval-uate how contaminants may interfere with the routes involved in estrogen synthesis during pregnancy. This has been traditionally assessed by measuring aromatase activity through the amount of tritiated water ((H2O)-H-3) formed during the aromatization of 1 beta-H-3-androst-4-ene-3,17-dione (H-3-AD). This work presents a greener and safer analytical approach for this purpose, which consists of the determination of the trace amounts of the steroids (estradiol, estrone, testosterone, and androstenedione) present in the culture medium. Turbulent flow chromatography coupled to liquid chromatography-tandem mass spec-trometry (TFC-HPLC-MS/MS) delivered the high selectivity and sensitivity (limits of detection between 2 and 5 pg/mL) required for these measurements. Moreover, its automation allows high-throughput of samples with minimum sample handling and achieves high precision in the analysis (relative standard deviation values < 6%). As a proof of concept, the method was applied to evaluate the effect of mono-haloacetic acid exposure on the steroid profile of JEG-3 cells. Iodoacetic acid showed an estrogenic effect (statistically significant increase of estradiol levels compared to unexposed cells) at the highest concen-tration level tested (0.5 mu M) that deserves further evaluation. (C) 2022 The Author(s). Published by Elsevier B.V.
      原文链接:
    • NSTL
    • Elsevier

    High throughput and very specific screening of anabolic-androgenic steroid adulterants in healthy foods based on stable isotope labelling and flow injection analysis-tandem mass spectrometry with simultaneous monitoring proton adduct ions and chloride adduct ions

    Zhang, Jun-WeiWu, De-QiaoWang, Zi-YueYu, Xin-Rui...
    8页
    查看更多>>摘要：In this work, a stable isotope labelling-flow injection analysis-tandem mass spectrometry (SIL-FIA-MS/MS) with simultaneous monitoring [M + H](+) and [M+ Cl](-) method was developed for very specific and high throughput screening of anabolic-androgenic steroids (AAS) illegally added to healthy foods. Initially, a simple centrifugation step was carried out for liquid samples, and for solid samples, a solid-liquid extraction step was conducted. Afterwards, batch chemical derivatization was carried out. After adding a certain amount of C-13(6)-3-NPH labelled AAS standards as the internal standards, it can be directly transferred for FIA-MS/MS analysis based on the no MS response characteristics of 3-NPH. The 3-NPH labelled AAS showed dual-polarity property, observing chloride adduct ion ([M + Cl](-)) in negative ion mode and proton adduct ion ([M + H](+)) in positive ion mode. The average time cost for pretreatment of each sample was less than 1 min by carrying out batch processing. The subsequent FIA-MS/MS detection enabled rapid and high throughput detection. The addition of C-13(6)-3-NPH-labelled AAS as internal standards can correct the matrix effect to achieve accurate quantitative analysis. The detection sensitivity was also improved by 2-5 folds after 3-NPH labelling. The limits of detection (LODs) in positive MRM mode were in ranges of 0.1-0.3 ng/mL. The validated method with simultaneous monitoring [M + H](+) and [M+ Cl](-) was validated in the range of 6.0-10 0 0 ng/mL with the linear coefficient (R-2 ) greater than 0.997. Satisfactory recoveries were found to be in ranges of 93.0-108.7%. The intra-day and inter-day RSDs were in the range of 3.5-9.9% and 5.1-14.1%, respectively. No changes in detection sensitivity of the mass spectrometry and no carry-over effects were found after numerous consecutive injections of AAS derivates. Compared with previously reported methods, the proposed method proved accurate, very specific, high throughput with good sensitivity. (C) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Diboronic acid assisted labeling and separation for highly efficient analysis of saccharides

    Li, XueBie, ZijunChen, Yang
    6页
    查看更多>>摘要：In this study, a diboronic acid assisted labeling and separation strategy was proposed for the efficient analysis of saccharides in real samples. The diboronic acid was first synthesized and characterized and then used as chemical labels for saccharides through boronate affinity. After labeling, the product was direct submitted to chromatographic analysis. The whole labeling procedure was organic solvent-free and could be accomplished within 1 h. Furthermore, the separation could be realized on the most commonly used chromatographic techniques (RPLC-UV). Taking glucose as an example, the established strategy pro-vided broad linear dynamics ranges (25-50 0 0 ng/mL) with acceptable correlation coefficients (R 2 > 0.98), substantial sensitivity (LOD: 5 ng/mL), high reproducibility (RSD < 6.7%) and excellent accuracy (Recovery: 98.2-99.8%). Finally, different saccharides were successfully analyzed in various complex samples, from tryptic glycans of glycoproteins to monosaccharides in traditional Chinese medicine. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Coupling of chiral and achiral stationary phases in supercritical fluid chromatography: Evaluating and improving retention prediction

    Riasova, PetraJac, PavelPolasek, MiroslavVander Heyden, Yvan...
    10页
    查看更多>>摘要：Isomers and stereoisomers are always challenging to separate. Column coupling may provide improved chromatographic selectivity, necessary for the separation of the compounds with similar chemical and structural properties. The relatively low viscosity of supercritical fluids, used as mobile phases allows for the coupling of several columns in series in supercritical fluid chromatography (SFC), without exceeding the pressure limits of the system. The aim of this study is to propose reliable prediction of the retention behaviour of analytes on a coupled column system, based on a limited number of initial analyses. The chiral compounds atenolol, ephedrine, propranolol, mianserin, labetalol and nadolol, besides the diastereomers quinine and quinidine, and the structural isomers of aminophenol and aminocresol were used as model analytes. The retention behaviour of the analytes was determined on the individual chiral columns Lux Cellulose-1, Lux Cellulose-2, Lux Cellulose-3, Lux Cellulose-4, Lux Amylose-2 and the achiral columns Luna NH2, Luna Silica, Synergi RP and FluoroSep RP. The mobile phase was composed of CO2 mixed with 20% (v/v) MeOH, which contained 0.1% (v/v) trifluoroacetic acid and 0.1% (v/v) isopropylamine. The retention factors of the analytes on coupled stationary phases were predicted, and subsequently compared to the experimentally obtained ones. Relative deviations of predicted and experimental retention factors were in range from 0.00% to 51.91%. Flow rate and back pressure of the screening conditions were adjusted to improve prediction precision on four column combinations, with varying success rates. The average relative deviations of retention factors were reduced to 2.84% -6.59% by adjusting flow rate, and to 2.30% -8.57% by adjusting back pressure. The most successful approach, flow rate adjustment, was then applied to select a column combination providing improved resolution of the structurally similar components of silymarin extract. (C) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Accurate determination of amino acids by quadruple isotope dilution-reverse phase liquid Chromatography-Tandem mass spectrometry after derivatization with 2-Naphthoyl chloride

    Er, Elif OzturkErarpat, SezinBodur, SuleymanGunkara, Omer Tahir...
    8页
    查看更多>>摘要：The determination of amino acids in biological samples is central to the diagnosis of inherited metabolic disorders and also gives significant information about the metabolisms in the cells and living body. The development of analytical method for reliable quantification of amino acids in biological samples is still challenging because of the polar nature of amino acids and complex nature of biological samples causing a high degree of interferences during analysis. In the present study, a pre-column derivatization method using 2-naphtoyl chloride combined with liquid chromatography-tandem mass spectrometry method was developed for the determination of 17 amino acids in human serum and urine matrices. Low detection limits were obtained in the range of 0.015 - 0.266 mu mol kg(-1) and acceptable recovery results were obtained in human serum and urine samples. Isotopically labelled (N-15 labelled) amino acids were spiked to standards and samples before derivatization to compensate for the analytical errors in the whole procedure. The combination of quadrupole isotope dilution strategy with the derivatization based reversed phase chromatography allowed to improve method accuracy and precision. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Methanetriyl-pi hydrogen bonding in nonpolar domains of supramolecular nanostructures: An efficient mechanism for extraction of carcinogenic polycyclic aromatic hydrocarbons from soils

    Dolores Sicilia, MariaRubio, SoledadAlgar, Lourdes
    9页
    查看更多>>摘要：Methanetriyl-pi hydrogen bonding (CH-pi HB) in nonpolar domains of supramolecular nanostructures is proposed here as a new mechanism to increase the extraction efficiency of aromatic compounds. The ap-proach is illustrated by the extraction of priority carcinogenic polycyclic aromatic hydrocarbons (CPAHs) in soils using supramolecular nanostructures of carboxylic acids with nonpolar domains consisting of hydrocarbon chains (C6-C10) dispersed in tetrahydrofuran (THF). The high concentration of CH-groups available in the supramolecular nanostructures (38.7-47.3 M) enabled the efficient extraction of CPAHs (recoveries between 89 and 106%), using a supramolecular solvent (SUPRAS) volume/soil amount ratio of 1.5 mu L mg(-1) and a simple and quick procedure (stirring for 15 min and centrifugation for 10 min). SUPRAS extracts were directly analysed by liquid chromatography-fluorimetry (LC-FL). No sample clean-up or solvent evaporation was required. Optimization of the composition of the nonpolar domains of the SUPRASs was carried out varying the length and concentration of the hydrocarbon chain of the carboxylic acid and the concentration of THF. Method detection limits were in the interval 0.07-0.4 mu g kg(-1). The rel-ative standard deviations (n = 18, CPAH concentration = 300 mu g kg(-1)), obtained under repeatability and reproducibility conditions, varied within the ranges 2.8-5.4% and 4.3-8.8%, respectively. The accuracy of the method was proved by analysing a certified reference material (CRM) from an industrial soil, con-taminated with priority CPAHs at concentrations at the mg kg(-1) level (BAM-U013c). The concentration of CPAHs found in soils taken in Southern Spain varied in the range 0.51-49 mu g kg(-1). The results here obtained demonstrate that CH-pi HB is a valuable mechanism for increasing the extraction of aromatic compounds from soils. (c) 2022 The Author(s). Published by Elsevier B.V.
      原文链接:
    • NSTL
    • Elsevier

    Suspect and non-target screening workflow for studying the occurrence, fate, and environmental risk of contaminants in wastewater using data-independent acquisition

    El-Deen, Asmaa KamalShimizu, Kuniyoshi
    11页
    查看更多>>摘要：A comprehensive suspect and non-target screening workflow based on liquid chromatography coupled to a quadrupole-time-of-flight mass spectrometer was developed for the detection and identification of contaminants in wastewater using data-independent acquisition. The suspect screening workflow could identify 74 compounds from different classes (mainly pharmaceuticals and pesticides), of which37 compounds were confirmed by reference standards.The remaining 37 compounds were tentatively identified based on MS/MS spectra match. The occurrence and elimination of the identified compounds were studied and discussed in detail. Furthermore, the confirmed compounds were quantified where pharmaceuticals had the greatest overall concentrations in all samples, followed by flame retardants. The non-steroidal antiandrogen, bicalutamide, was detected at the highest concentration (843.9 to 3838 ng/L) at the wastewater effluents, where the flame retardant, tris(2-butoxyethyl) phosphate, exhibited a concentration in the range of 337.2 to 1304.6 ng/L. Consequently, the environmental toxicity and risk of the confirmed compounds were investigated. The pharmaceutical, telmisartan, with the insecticide, fipronil exhibited high-risk quotients ( 60 0-140 0 and 102-290, respectively), demonstrating their potential toxicity at ecologically relevant amounts. Finally, multivariate analysis was applied to evaluate the efficiency of wastewater treatment . Principal component analysis was able to clearly discriminate between influent and effluent samples, demonstrating an effective treatment process.. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier