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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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    Progress of chiral ligand-exchange capillary electrophoresis for enantioseparation

    Qiao J.Qi L.
    5页
    查看更多>>摘要：? 2022Chiral ligand exchange capillary electrophoresis (CLE-CE) has become an area of tremendous interest in chiral separation science, particularly in life science and pharmaceutical, due to its notable simplicity, tunable migration order, and outstanding performance. This approach effectively separates enantiomers in drugs, food products and bio-samples. Nevertheless, the main challenges in CLE-CE are the limited chiral ligand-species, unclear mechanism of thermodynamic enantioseparation and unsatisfactory enantioseparation efficiency, which restrict its applications. Designing desirable chiral ligand-species and exploring profitable central metal ions are considered to be efficient strategies for addressing these obstacles, which can improve the performance of CLE-CE and expand its application in living bio-systems. This review introduces the concept of desirable chiral ligand species and highlights the latest CLE-CE research in the last decade, with special emphasis on boosting its enantioseparation efficiency and expanding its cutting-edge application. Moreover, further research in the CLE-CE field is prospected
      原文链接:
    • NSTL
    • Elsevier

    Preparation and evaluation of a chiral porous organic cage based chiral stationary phase for enantioseparation in high performance liquid chromatography

    Li K.Xiong L.-X.Wang Y.Zhang Y.-P....
    5页
    查看更多>>摘要：? 2022 Elsevier B.V.Porous organic cages (POCs) are a new kind of porous molecular materials, which have gained widespread interest in many fields due to their intriguing properties, including excellent molecular solubility, inherent molecular cavity and rich host-guest chemistry. To date, many chiral POCs have been explored as chiral stationary phases (CSPs) for gas chromatographic (GC) separation of enantiomers. However, the applications of chiral POCs for high performance liquid chromatography (HPLC) enantiomeric separation is extremely rare. In this study, we report the construction of thiol-ene click reaction for the preparation of CSP for HPLC by using a [4+8]-type chiral POC NC4-R as chiral selector. The fabricated CSP showed good chiral resolution performance not only in normal-phase HPLC (NP-HPLC) but also in reversed-phase HPLC (RP-HPLC). Seventeen and ten racemates were well resolved in the two separation modes, respectively, including ketones, esters, alcohols, phenols, amines, ethers, organic acids, and amino acids. Moreover, the fabricated column also shows good chiral recognition complementarity to two popular chiral HPLC columns (Chiralpak AD-H and Chiralcel OD-H columns) and previously reported chiral POC NC1-R-based HPLC column, which can resolve some racemates that unable to be resolved by the two commercially available chiral HPLC columns and NC1-R-based column. The relative standard deviation (RSD) values (n = 4) of retention time and resolution (Rs) of analytes separated on the column were less than 0.3 % and 0.5 % after it was subjected to different injections, showing the good reproducibility and stability of the NC4-R-based column. This work demonstrated high potentials of chiral POCs for HPLC enantioseparation and the applicability of chiral POC-based HPLC columns can be broadened by developing more chiral POCs with diverse structures as chiral selector for HPLC.
      原文链接:
    • NSTL
    • Elsevier

    A core-shell structured magnetic sulfonated covalent organic framework for the extraction of benzoylureas insecticides from water, pear juice and honey samples

    Liu Z.Duan T.Guo Y.Liu W....
    5页
    查看更多>>摘要：? 2022 Elsevier B.V.Three magnetic covalent organic frameworks (named M-TpPa-SO3Na, M-TpPa-SO3H and M-TpPa) were prepared by the solvothermal synthesis method with 1,3,5-trimethylphenol (TP) and either 2-sulfo-1,4-phenylenediamine (Pa-SO3H) or p-phenylenediamine (Pa) as monomers. Among them, the M-TpPa-SO3Na possessed relatively high hydrophilicity, good magnetic responsiveness, and high affinity for the benzoylureas (BUs) insecticides. It was then explored as the magnetic solid-phase extraction adsorbent for the extraction of six BUs (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, flufenoxuron and chlorfluazuron) from water, pear juice and honey samples prior to high-performance liquid chromatography with ultraviolet detection. Under the optimized experimental conditions, a good linearity was achieved within the concentration range of 0.27-40.0 ng mL?1 for water sample, 0.47-30.0 ng mL?1 for pear juice sample, and 2.70-200.0 ng g?1 for honey sample. The limits of detection for the analytes were 0.08-0.11 ng mL?1 for water sample, 0.14-0.19 ng mL?1 for pear juice sample and 0.80-1.00 ng g?1 for honey sample. The method recoveries for spiked samples were in the range of 85.0%-111.0% with the relative standard deviations less than 8.8%. The developed method was successfully used for the determination of the BUs in water, pear juice and honey samples.
      原文链接:
    • NSTL
    • Elsevier

    Magnetic solid-phase extraction method with modified magnetic ferroferric oxide nanoparticles in a deep eutectic solvent and high-performance liquid chromatography used for the analysis of pharmacologically active ingredients of Epimedium folium

    Zhang Y.Li Z.Li L.Gao M....
    5页
    查看更多>>摘要：? 2022 Elsevier B.V.A novel magnetic adsorption nanomaterial was synthesized by the copolymerization of a deep eutectic solvent (DES) and chitosan (CS)-modified Fe3O4 particles. This material was proposed for the magnetic solid-phase extraction (MSPE) of flavonoids from an aqueous extract solution of herbal Epimedium folium without pretreatment. Coupled with high-performance liquid chromatography (HPLC), a rapid, environmentally friendly, and efficacious method was established and successfully applied for the enrichment, separation, and quantification of five quality marker flavonoids (viz. icariin, epimedin A, epimedin B, epimedin C, and baohuoside Ⅰ, respectively) in herbal E. folium collected from four species and 18 habitats. In addition, the physicochemical properties and morphology of Fe3O4-CS-DES were characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, X-ray diffraction, and vibrating sample magnetometry. Furthermore, key parameters, including adsorbent amount, elution solvent, and desorption factor, were optimized. Under the optimal experimental conditions, the five flavonoids were adsorbed rapidly on MSPE, which were released easily using methanol-acidified formic acid. A reversed-phase C18 column with gradient mobile phases comprising acetonitrile and formic acid water was used for analyte separation and elution. Limits of detection for the five analytes ranged from 0.5 to 2.1 ng mL?1. Coefficients of determination in analyses ranged from 0.99994 to 0.99999. Intra-day and inter-day precision ranged from 0.75 to 5.18% (n = 6) and from 2.88 to 7.52% (n = 3), respectively. Recoveries of the five analytes ranged from 80 to 110%, with relative standard deviation values of less than 10%. To the best of our knowledge, as a new adsorbent, Fe3O4-CS-DES nanoparticles were synthesized and used for the first time for the preconcentration and separation of flavonoids. This study provided a new approach for the enrichment and detection of Epimedium flavonoids in real samples.
      原文链接:
    • NSTL
    • Elsevier

    Strain-specific quantification of probiotic Bacillus subtilis in feed by imaging high-performance thin-layer chromatography

    Kruse S.Becker S.Morlock G.E.Pierre F....
    5页
    查看更多>>摘要：? 2022 Elsevier B.V.The European Union has banned the use of antibiotic growth promoters in animal production, which has led to increased use of probiotic microorganisms. These feed additives result in higher costs for farmers, which is why the demand for a quality control system to quantify probiotics in feeds has increased in recent years. Imaging high-performance thin-layer chromatography (HPTLC) was proven to be a robust method for determining the probiotic Bacillus subtilis DSM 29784 strain based on the production of selective bacterial metabolites and thus characteristic metabolite pattern. However, to quantify the specific probiotic strain in the feed, identification of a strain-specific metabolite not produced by genetically very similar bacteria is necessary. Compared to five bacteria with high genetic similarity, a strain-specific metabolite was formed in the probiotic bacteria by a two-step cultivation procedure. Among others, antimicrobial properties were found for this metabolite, which indicated probiotic activity. The hyphenation of normal-phase HPTLC with reversed-phase high-performance liquid chromatography diode array detection and high-resolution mass spectrometry allowed the preliminary assignment of this strain-specific metabolite to the molecular formula C35H44N6O2 (580.3527 Da). This metabolite, produced each time via an upstream cultivation process to generate the standard levels, was used for the quantification of probiotic active cells in the feed. Data on selectivity, linearity, detection limit, recovery, and precision have shown the good performance of the method.
      原文链接:
    • NSTL
    • Elsevier

    Preparation of reversed-phase/boronate affinity mixed-mode restricted access materials with zwitterionic polymer outer layers and its extraction properties

    Li Y.Ma X.Gong B.Guo S....
    5页
    查看更多>>摘要：? 2022High-selectivity and high-exclusion restricted access materials (RAMs) benefit the demands of complex biological samples. In this study, mixed-mode-adsorption RAMs bearing zwitterionic polymer brushes as their outer layers were proposed. The reversed-phase/bronate affinity (RP/BA) mixed-mode adsorption layers on the surface of the silica gel were first formed by surface-initiated atom transfer radical polymerization (SI-ATRP) employing styrene (St) and 4-vinylphenylboronic acid (4-VPBA) as comonomers Afterward, zwitterionic poly(sulfobetaine methacrylate, SBMA) was grafted via another SI-ATRP reaction to establish the external hydrophilic layer. The selectivity of the developed Sil@poly(St-co-4-VPBA)@poly(SBMA) RAMs was examined employing different analytes (benzenes, tetracyclines, neurotransmitters, β-agonists, and their structural analogs), the results revealed the preferential adsorption of substances bearing phenyl and cis-diol groups owing to the multiple interactions (hydrophobic, π-π and BA forces) caused by the RAMs with RP/BA mixed-mode adsorption mechanism. On the other hand, the synergistic effect of the strong-hydrophilicity and high-density zwitterionic poly(SBMA) could efficiently promote the exclusion of RAMs. Moreover, the experimental data revealed that > 99% of bovine serum albumin (BSA, 1 g L–1) could be excluded, although the tetracycline (50 μg L–1) was completely adsorbed, indicating the maximized adsorption capacity of the RAMs toward small molecules after the efficient exclusion of protein interference. Solid-phase extraction (SPE) employing the developed Sil@poly(St-co-4-VPBA)@poly(SBMA) RAM coupled with high-performance liquid chromatography (HPLC) was successfully employed to determine the tetracycline content of a milk sample. The established method exhibited satisfactory linearity (10–700 μg L–1), high recovery (93.1%–108.6%) and good precision (2.6%–8.4%). Finally, our proposed method for synthesizing RAMs could efficiently boost the adsorption selectivity and restricted access function of RAMs, thereby promoting their application in analyzing biological samples.
      原文链接:
    • NSTL
    • Elsevier

    Development of peptide ligands for the purification of α-1 antitrypsin from cell culture fluids

    Prodromou R.Moore B.Kilgore R.Shastry S....
    5页
    查看更多>>摘要：? 2022α-1 antitrypsin (AAT) deficiency, a major risk factor for chronic obstructive pulmonary disease, is one of the most prevalent and fatal hereditary diseases. The rising demand of AAT poses a defined need for new processes of AAT manufacturing from recombinant sources. Commercial affinity adsorbents for AAT purification present the intrinsic limitations of protein ligands – chiefly, the high cost and the lability towards the proteases in the feedstocks and the cleaning-in-place utilized in biomanufacturing – which limit their application despite their high capacity and selectivity. This work presents the development of small peptide affinity ligands for the purification of AAT from Chinese hamster ovary (CHO) cell culture harvests. An ensemble of ligand candidates identified via library screening were conjugated on Toyopearl resin and evaluated via experimental and in silico AAT-binding studies. Initial ranking based on equilibrium binding capacity indicated WHAKKSKFG- (12.9 mg of AAT per mL of resin), WHAKKSHFG- (16.3 mg/mL), and KWKHSHKWG- (15.8 mg/mL) Toyopearl resins as top performing adsorbents. Notably, the fitting of adsorption data to Langmuir isotherms concurred with molecular docking and dynamics in returning values of dissociation constant (KD) between 1 – 10 μM. These peptide-based adsorbents were thus selected for AAT purification from CHO fluids, affording values of AAT binding capacity up to 13 gram per liter of resin, and product yield and purity up to 77% and 97%. WHAKKSHFG-Toyopearl resin maintained its purification activity upon 20 consecutive uses, demonstrating its potential for AAT manufacturing from recombinant sources.
      原文链接:
    • NSTL
    • Elsevier

    Functionalization of chitosan by metformin, nickel metal ions and magnetic nanoparticles as a nanobiocomposite for purification of alkaline phosphatase from hen's egg yolk

    Eivazzadeh-Keihan R.Choopani L.Gorab M.G.Kashtiaray A....
    5页
    查看更多>>摘要：? 2022In this study, a novel and green chitosan-metformin/NiCl2/Fe3O4 nanobiocomposite was synthesized and used to purify alkaline phosphatase (ALPs) from hen's egg yolk. For this purpose, after functionalization of the chitosan biopolymer by terephthaloyl chloride-metformin ligand, the coordination with Ni(II) and magnetization process were performed. The structure and properties of the synthesized nanobiocomposite were then evaluated by using analyzes such as FT-IR, EDX, FE-SEM, XRD, TGA and VSM. Purification of ALPs with chitosan-metformin/NiCl2/Fe3O4 nanobiocomposite is a fast, reusable and cost-effective method. By this protocol, 62% purification efficiency was obtained and the synthesized nanobiocomposite was not attached to other proteins in hen's egg yolk. ALPs was obtained approximately in the pure form and the purification process was evaluated using SDS-PAGE. The reusability of nanobiocomposites was evaluated and a slight decrease in adsorption capacity was observed after 4 cycles.
      原文链接:
    • NSTL
    • Elsevier

    Pseudophase-to-solvent microextraction for in-line sample concentration of anionic analytes in capillary zone electrophoresis

    Yu R.B.Quirino J.P.
    5页
    查看更多>>摘要：? 2022We present pseudophase-to-solvent microextraction (PSME) as a simple pressure-driven in-line sample concentration technique in capillary zone electrophoresis (CZE) for small organic anions. The developed technique is like solid-phase extraction; however, the chromatographic phase is a pseudophase, i.e., in-situ cetyltrimethylammonium bromide (CTAB) interfacial micelles. A large volume of sample (e.g., > 12 capillary volumes) prepared in [CTAB] ～critical micelle concentration was injected into the capillary. The elution and enrichment of analytes trapped in the CTAB coating was facilitated by the high concentration of methanol in the background solution, which was introduced from the outlet end. Co-electroosmotic flow CZE was conducted after the concentrated analytes reached the tip of the inlet. Parameters such as sample loading time and elution time were optimised. Under optimised conditions, the SEFs of 187–573 achieved for the model anions (4-nitrophenol, 4-vinylbenzoic acid, mecoprop, indoprofen, sulfamethizole and sulindac) were comparable to previously reported off-line microextraction techniques. The calculated LOD (S/N = 3), LOQ (S/N = 10), intra-/inter- (n = 6/n = 9, 3 days) day repeatability and linearity (R2s) values in PSME-CZE were 4.2–20.1 ng/mL, 13.8–67.1 ng/mL, 5%, 10% and > 0.990, respectively. The PSME-CZE of fortified urine samples showed % recovery values of 93–108% with %RSDs (n = 3) of 4–10% for the model analytes.
      原文链接:
    • NSTL
    • Elsevier