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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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    A beta-cyclodextrin sorbent based on hierarchical mesoporous silica for the determination of endocrine-disrupting chemicals in urine samples

    Belenguer-Sapina, CarolinaAmoros, PedroPellicer-Castell, EnricEl Haskouri, Jamal...
    9页
    查看更多>>摘要：In the present work, a method for the determination of parabens and bisphenol A in urine samples has been developed. For this purpose, a novel hierarchical mesoporous silica doped with beta-cyclodextrin was developed and used as a sorbent for preconcentration and clean-up step, before analyte determination by liquid chromatography coupled to mass spectrometry detector. Disordered silica materials were also synthesized for comparison purposes. All materials were characterized by electron microscopy, X-ray diffraction, porosimetry, nuclear magnetic resonance, thermogravimetric analysis, elemental CNH analysis, and confocal microscopy, and the attachment of cyclodextrins has been proved as well as their uniform distribution in the resulting material. After the optimization of several protocol parameters, good analytical features were achieved, including recoveries in the range of 96-109% for all analytes, as well as relative standard deviations between 8 and 24%. Also, limits of quantification in the range of 0.003-0.19 mu g L-1 were obtained in all cases. The developed method was applied to the determination of parabens and bisphenol A in real urine samples in comparison with a reference method using C18 cartridges, including the correction with creatinine content. Target analytes were detected in all analysed samples, with being BPA the most detected compound. (C)& nbsp;2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Liquid chromatography-tandem mass spectrometry based quantification of arginine metabolites including polyamines in different sam ple matrices

    Langner, MathiasMateska, IvonaBechmann, NicoleWielockx, Ben...
    10页
    查看更多>>摘要：The conditionally essential amino acid arginine and its metabolic products play an important role in different biological processes, such as metabolic regulation of the immune response, including macrophage activation and polarization and regulation of T cell function. Furthermore, the polyamine spermidine has a role in aging and age-related diseases. Additionally, altered polyamine metabolism may be associated with neurodegenerative diseases, while polyamine levels may present useful biomarkers associated with severity of Parkinson's disease or with progression of non-alcoholic fatty liver disease. In the present study, a simple, derivatization-free hydrophilic interaction liquid chromatography based tandem mass spectrometry (LC-MS/MS) method is described, that allows the accurate quantification of arginine and related amine, polyamine and acetylated polyamine metabolites in different experimental sample matrices, such as cell lysates, cell culture supernatants and tissues. Ten arginine metabolites, including citrulline, agmatine, ornithine, putrescine, spermidine, spermine, N1-acetylspermidine, N1-acetylspermine, N1,N12diacetylspermine and arginine in conjunction with the metabolic cofactors S-adenosylhomocysteine and S-adenosylmethionine are simultaneously analyzed within a total LC-MS/MS run time of 9.5 min. The assay is suitable to quantify concentration ranges over multiple orders of magnitude for all metabolites with averaged accuracies observed at 103.2% +/- 6.8%, 99.0% +/- 4.2% and 100.4% +/- 4.3% in cell lysates, cell culture supernatant and tissue extracts, respectively. Inter-day coefficients of variation ranged from 5.9 to 14.8% in cell lysates, 6.7 to 14.6% in cell culture supernatants and 5.3 to 12.0% in tissue extracts. The method was successfully applied to cell culture systems of different origin as well as different murine tissues and organs. The herein described LC-MS/MS method provides a simple tool for a fast and simultaneous analysis of arginine metabolites, including polyamines and their respective metabolic cofactors. Assay performance characteristics demonstrate suitability for applications in different experimental and preclinical settings.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Building machine-learning-based models for retention time and resolution predictions in ion pair chromatography of oligonucleotides

    Enmark, MartinHaggstrom, JakobSamuelsson, JorgenFornstedt, Torgny...
    10页
    查看更多>>摘要：Support vector regression models are created and used to predict the retention times of oligonucleotides separated using gradient ion-pair chromatography with high accuracy. The experimental dataset consisted of fully phosphorothioated oligonucleotides. Two models were trained and validated using two pseudo orthogonal gradient modes and three gradient slopes. The results show that the spread in retention time differs between the two gradient modes, which indicated varying degree of sequence dependent separation. Peak widths from the experimental dataset were calculated and correlated with the guanine cytosine content and retention time of the sequence for each gradient slope. This data was used to predict the resolution of the n - 1 impurity among 250 0 0 0 random 12-and 16-mer sequences; showing one of the investigated gradient modes has a much higher probability of exceeding a resolution of 1.5, particularly for the 16-mer sequences. Sequences having a high guanine-cytosine content and a terminal C are more likely to not reach critical resolution. The trained SVR models can both be used to identify characteristics of different separation methods and to assist in the choice of method conditions, i.e. to optimize resolution for arbitrary sequences. The methodology presented in this study can be expected to be applicable to predict retention times of other oligonucleotide synthesis and degradation impurities if provided enough training data. (c) 2022 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license ( http://creativecommons.org/licenses/by/4.0/ )
      原文链接:
    • NSTL
    • Elsevier

    Automated method for short-chain aldehydes emission measurement by dynamic solid-phase microextraction on-fiber derivatization GC-MSD coupled with a flow-cell

    Sai, TingDuan, ShuyuWinniford, BillZhang, DeGang...
    10页
    查看更多>>摘要：A novel automated method was developed to test short-chain aldehyde emissions using a chamber and a flow-cell coupled with a dynamic solid-phase microextraction (SPME) on-fiber derivatization technique. Calibration curves of short-chain aldehydes were developed for quantitation of target analytes, includ-ing formaldehyde, acetaldehyde, propionaldehyde, and acrolein emitted from the chamber outlet. The linearity range for the aldehydes was 0.8 to 2130.0 mu g/m(3). The limits of quantitation (LOQ) for various aldehydes ranged from similar to 0.2 - 1.9 mu g/m(3). By using this method, emission rate curves are measured with an automated system. Compared with a traditional 2,4-dinitrophenyl hydrazine (DNPH)-high performance liquid chromatography (HPLC) method for aldehyde emission measurement, this method provided an automated technique to study the emission of short-chain aldehydes from multiple samples in one experiment. Furthermore, by using dynamic SPME coupled to an on-fiber derivatization technique, the repeatability and sensitivity of the method is comparable and even better than traditional techniques. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Simultaneous solvent extraction and quantification of eleven amine compounds related to Chemical Weapon Convention in soils via hydrophilic interaction liquid chromatography-tandem mass spectrometry

    Yang, YangLiu, Chang-CaiJiang, Pei-YuYuan, Ling...
    13页
    查看更多>>摘要：The detection of Chemical Weapon Convention (CWC)-related amine compounds including the precursors or degradation products of V-type organophosphorus nerve agent, nitrogen mustard and 3-quinuclidinyl benzilate is an important aspect for verifying their intact chemical warfare agents. This work focuses on the development of a novel formulation for the simultaneous solvent extraction of eleven CWC-related amine compounds, from the four-type soil matrices including environmental standard soil, sand, clay, and loam. Extracts were well separated on the hydrophilic interaction liquid chromatography (HILIC) and then detected by MS/MS multiple reaction monitoring mode. The type and component of solvent mixtures were optimized to cover a wide range of polarity over all eleven amine compounds with high extraction efficiencies. Extraction parameters, such as the proportion of methanol, water and NH 4 OH, the times and the period of extraction, and volumes of extraction solution were optimized. The results indicated that a mixed solvent of methanol/water (44:53, v/v) in 3.0% NH 4 OH was the optimal formulation for extraction of all 11 analytes with high mean extraction recoveries (64.4-96.1%). Specificity and sensitivity were well improved by the good separation of 11 analytes from four-type soil matrices using these optimized HILIC parameters. This method was fully validated for each analyte in four soil matrices. The linear range of 11 analytes was 0.50/0.75-50 0 ng center dot g -1 with correlation coefficient ( R 2 ) >0.990, and intra/inter-day accuracies were 70.3-125% with relative standard deviation (RSD) <19.3%. Limit of detection (LOD) of 11 analytes ranged from 0.01 to 0.5 ng center dot g -1 , which was far lower than those reported in previous studies. The built method accomplishes simultaneously quantitative and trace measurement of all eleven CWCrelated amine compounds within a single solvent extraction and detection. It only takes a small amount of soil samples and possesses the highest sensitivity over all previous methods. This study provides an optional recommended operating procedure for determination of CWC-related amine compounds in four typical types of complex soils during chemical weapons verification. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Metal-organic framework-based magnetic dispersive micro-solid-phase extraction for the gas chromatography-mass spectrometry determination of polycyclic aromatic compounds in water samples

    Fornari, FabioBianchi, FedericaCasoli, FrancescaBacchi, Alessia...
    11页
    查看更多>>摘要：A magnetic hybrid material based on the use of the mixed-ligand Metal-Organic Framework (MOF) PUM198 is proposed for the magnetic dispersive micro solid-phase extraction (MD mu SPE) of the 16 poly cyclic aromatic hydrocarbons (PAHs) included in the US-EPA priority pollutants list. PUM198 is a thermally robust MOF characterized by a doubly interpenetrated microporous framework in which Zn2+ ions and carboxylate groups define 2D planes that are pillared by a bis-pyridine-bis amide ligand containing a biphenyl scaffold. PUM198 revealed to be ideal to adsorb PAHs efficiently through non-covalent interactions. A Plackett-Burman Design followed by a Central Composite Design and the multicriteria method of the desirability functions were applied to find the optimal conditions for the extraction of the investigated PAHs, resulting in a reduced solvent consumption, i.e., 50 mu L of solvent per extraction for 5 mL of sample, approximatively 3-20 times lower than those reported in previous studies, thus satisfying the principles of green analytical chemistry. Method validation proved the reliability of the method for the determination of PAHs at trace level, obtaining detection limits in the 6.7-27 ng/L range, good precision with RSDs(%) lower than 19% and recovery rates in the 99 ( +/- 13)-126 (+/- 8)% range near the quantitation limit. Finally, the applicability of the method was demonstrated by analyzing underground water samples taken from contaminated sites C()& nbsp;2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Core-shell MOFs-based composites of defect-functionalized for mixed-mode chromatographic separation

    Si, TiantianWang, LichengZhang, HaixiaLu, Xiaofeng...
    8页
    查看更多>>摘要：The micropores of the metal-organic frameworks (MOFs) endow with the advantages of size selectivity and large specific surface area, etc., but they limit their applications toward the control of diffusion and transport processes. Here, we report a strategy to prepare the hierarchical porous material, functional defect, which allows incorporation of L-Cysteine in the MOF by defect-loading. Silica microspheres were modified with these materials to form core-shell composites and used as mixed-mode stationary phases for chromatographic separations. Compared with the traditional MOFs-based stationary phase, it exhibited superior efficiency and selectivity for separation of various analytes and highlighted the role of defect of MOFs and function of L-Cysteine. In addition to the rapid separation of hydrophobic compounds, the stationary phase showed great potential in the separation of hydrophilic analytes, especially for separation of ten carbohydrates and eight sulfonamides. It showed excellent chromatographic reproducibility and stability, and the repeatability of preparation was investigated by relative standard deviations of retention time and/or column efficiency of objective compounds, which was among different batches less than 1.81%. This demonstration provided deep understanding of separation mechanism between MOF-based composites with functional defect and analytes, and stimulated the wide applications of such defective MOFs complexes in separations and analysis.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Kinetic and molecular insight into immunoglobulin G binding to immobilized recombinant protein A of different orientations

    Chu, XinshuangYang, XuehuiShi, QinghongDong, Xiaoyan...
    11页
    查看更多>>摘要：Mechanistic understanding of immunoglobulin G (IgG) binding to protein A is crucial for the design and development of high-performance protein A chromatography. In this work, the IgG binding domain (Z) of protein A from Staphylococcus aureus was genetically modified by introducing a cysteine residue at the N-terminus (Cys-Z) or a cysteine-lysine dipeptide at the C-terminus (Z-Cys), and the two ligands were used to unravel the IgG binding mechanism by means of binding kinetics and different single molecule measurements. Surface plasma resonance (SPR) measurement of the binding kinetics of mouse myeloma IgG2a (mIgG2a) to the two ligands indicated that oriented ligand immobilization significantly increased the association rate constant of mIgG2a, and Z-Cys had the highest binding affinity to mIgG2a among the three ligands (Cys-Z, Z-Cys and Z). This was attributed to the synergistic contribution of the high association rate constant and low dissociation rate constant to mIgG2a. Furthermore, quartz crystal microbalance with energy dissipation monitoring (QCM-D) measurement provided the maximum adsorption densities of IgGs on the Z-Cys-immobilized chip as zeta potentials of IgGs were nearly zero. The QCM-D investigation revealed that the adsorbed layer was dependent on ligand type and density, and IgG. Moreover, Z-Cys and Cys-Z induced IgG binding in flipped orientations, as evidenced by the antigen-antibody reaction. Finally, rectangular DNA origami tiles were introduced to analyze the molecular orientation of adsorbed IgG. Single-molecule imaging showed that mIgG2a was associated with flexible Z-Cys on the tiles predominantly in side-on and end-on orientations. The research has provided molecular insight into the binding mechanism of IgG molecules at liquid-solid interfaces and would help design new protein A-based ligands and high-capacity adsorbents.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Preparation and application of polystyrene-divinylbenzene sorbent with weak cation-exchange character for the selective extraction of illicit drugs in environmental water

    Ning, HongyuFan, YileiLiu, HuijunHuang, Zhongping...
    12页
    查看更多>>摘要：A B S T R A C T A novel mixed-mode weak cation-exchange sorbent (PS-DVB-WCX-II) was prepared by the modification of polystyrene-divinylbenzene with mercaptosuccinic acid for the selective extraction of illicit drugs in environmental water. The PS-DVB-WCX-II was synthesized through the Friedel-Crafts acylation reaction on the surface of polystyrene-divinylbenzene, followed by nucleophilic substitution reaction and thiolene click reaction. The sorbent can selectively absorb illicit drugs through the reverse-phase interactions provided by benzene ring on the polymer backbone and the ion-exchange interactions provided by functional group (-COOH). As compared with the extraction performance of three commercial SPE cartridges, it was found that the prepared sorbent had better adsorption performance with the recovery values between 84.1% and 106.0% for the selected 11 illicit drugs under the optimized SPE conditions. Illicit drugs in environmental water were extracted by the sorbent, prior to the detection of UHPLC-MS/MS. Two quantitative methods were established respectively for the detection of 11 illicit drugs in different matrices of river water and wastewater. Both methods had good determination coefficient (r 2 > 0.992) in the range of 0.5-50 ng/L, 2.5-250 ng/L, 5-500 ng/L, and low limits of detection (S/N = 3) of 0.17-1.67 ng/L. In the real wastewater samples, the concentration of morphine was 18.3-126.3 ng/L, and the methamphetamine was 12.7-27.4 ng/L. Meanwhile, PS-DVB-WCX-II was compared with Oasis MCX and Oasis HLB in the detection of real wastewater samples. The results revealed that PS-DVB-WCX-II and Oasis MCX had better performance in absorbing methamphetamine than Oasis HLB, and PS-DVB-WCX-II had better ability to remove the matrix. The results suggested that the prepared weak cation-exchange sorbent had the potential in the application of illicit drug detection in environmental water.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Formation of trifluoroacetic artefacts in gas chromatograph injector during Cannabidiol analysis

    Holowinski, PiotrTypek, RafalDawidowicz, Andrzej L.Rombel, Michal...
    8页
    查看更多>>摘要：The knowledge of compounds stability in the process of sample preparation for analysis and during analysis itself helps assess the accuracy and precision of estimating their concentration in tested samples. The present paper shows that a significant amount of CBD present in the blood/plasma sample analyzed by means of GC transforms in the hot GC injector not only to 9 alpha-hydroxyhexahydrocannabinol, 8-hydroxy-iso-hexahydrocannabinol, delta-9-tetrahydrocannabinol, Delta 8-tetrahydrocannabinol, and cannabinol but also to the trifluoroacetic esters of Delta 9-THC and Delta 8-THC, when trifuoroacetic acid is used as protein precipitation agent. The amount of those newly revealed CBD transformation products depends on the GC injector temperature and on the extrahent type when extracts of the supernatants centrifuged from human plasma samples are analyzed after their preliminary protein precipitation by trifuoroacetic acid. Although trifuoroacetic acid as a protein precipitating agent has many disadvantages, it is quite often used for this purpose due to its very high protein precipitation efficiency. The results presented in the study demonstrate why the use of trifuoroacetic acid for plasma samples deproteinization should be avoided when CBD is determined by GC. (c) 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
      原文链接:
    • NSTL
    • Elsevier