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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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    The impact of endotoxin masking on the removal of endotoxin during manufacturing of a biopharmaceutical drug product

    Wespel, MartinaGeiss, MelanieNagele, MatthiasCombe, Stephanie...
    10页
    查看更多>>摘要：Endotoxins are a highly pyrogenic and immunogenic contaminant of bacterial origin that must be avoided during the manufacturing of biopharmaceutical products to ensure safety and efficacy. Low endotoxin recovery, also known as a masking effect, is defined as the ability to detect < 50% [21] of the expected endotoxin in an endotoxin assay. Masking can be caused by the ability of endotoxins to build aggregates, bind to the protein or organise in micelles or vesicles that in turn inhibit detection of the endotoxin in the solution being tested. Therefore, a masking effect can result from physical parameters of the molecule being tested or from the buffer/environmental conditions of the solution the molecule is in. This can subsequently lead to the underestimation of endotoxin contaminations and lead to a potential false negative test. Tight control over the effectiveness of the downstream process and the use of well-characterised endotoxin testing assays are needed to ensure optimal endotoxin removal. This manuscript demonstrates the capacity to remove the endotoxins within a proven acceptable range by also controlling and evaluating the potential masking effects during downstream process at ambient temperature and also during sample storage condition until the analyse was performed. The endotoxin removal study (ERS) is divided in the initial part to evaluate the process buffers and the conditions of the molecule to avoid the underestimation of endotoxins in process samples in advance. This pre-study is a necessary prerequisite to evaluate the results after the endotoxin spiked downstream unit operations. With those aspects, the removal capacity can be demonstrated. A study was carried out to characterise the endotoxin removal capability of the purification process including controlling of masking effects. The endotoxin removal capacity on ion exchange chromatography and during ultrafiltration/diafiltration unit operations of the downstream processing of an immunoglobulin G1 antibody was conducted using various process parameters to understand their impact on endotoxin removal. In the small-scale study, the processing steps from each tested unit operation were spiked with Escherichia coli endotoxins. The potential masking effect during purification was addressed by controlling the hold time by spiking studies of the different generated pools at ambient temperature. By conducting a masking study, all generated protein pools (flow-through/wash, eluate and regeneration pools) had no masking effect caused through sample handling prior to analysis. Overall, this study showed that endotoxins could be successfully removed by anion exchange chromatography. A partial removal could be achieved by cation exchange chromatography and endotoxins could not be removed with ultrafiltration/diafiltration. (c) 2022 The Authors. 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

    Noninvasive method for determination of immobilized protein A

    Podgornik, AlesMravljak, RokStantic, MetkaBizjak, Ozbej...
    7页
    查看更多>>摘要：The pH transition method, developed for the determination of the ion-exchange group density on chromatographic stationary phase, was used for the quantification of immobilized protein A. Monolithic epoxy polyHIPE and particulate CNBr-Sepharose supports were used for immobilization. A lactate buffer was selected, having a buffer capacity peak approximately 0.5 pH units below the maximum buffer capacity of protein A. The pH transition measurements were performed at pH 4.3, where protein A exhibits maximum buffer capacity, with a lactate buffer concentration of 1 mM for protein A immobilized on polyHIPE monoliths and of 5 mM for protein A immobilized on CNBr-Sepharose. The pH transition height and full width at half maximum for the particulate support and the height for the polyHIPE matrix, showed a linear correlation with the amount of immobilized protein A determined from the absorbance difference before and after immobilization for both supports. The developed method allows a simple, non-invasive online determination of immobilized protein A using biological buffers, even for chromatographic columns with an amount of immobilized protein A as low as 0.25 mg. In addition, its sensitivity and duration can be easily adjusted by varying the buffer concentration and pH.(c) 2022 The Authors. 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

    Comparison of three stationary phases in the separation of polyphenyls by liquid chromatography

    Brown, C. L.Dornan, L. M.Muldoon, M. J.Hembre, R. T....
    6页
    查看更多>>摘要：We present herein new analytical protocols for the separation and structural elucidation of polyphenyls. Three commercially available chromatographic stationary phases are compared in the separation of these non-polar, unfunctionalized, positional isomers. Baseline separation of nine terphenyl and quaterphenyl isomers is achieved in under ten minutes using a rapid gradient elution HPLC method. Complete separation of these, and a further five polyphenyls, is demonstrated. We finally present a linear correlation between solvent accessible surface area and the retention times of these closely related compounds. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Analytical method to monitor contaminants of emerging concern in water and soil samples from a non-conventional wastewater treatment system

    Huidobro-Lopez, BlancaLopez-Heras, IsabelAlonso-Alonso, CovadongaMartinez-Hernandez, Virtudes...
    15页
    查看更多>>摘要：Nonconventional wastewater treatments, such as vegetation filters (VFs), are propitious systems to attenuate contaminants of emerging concern (CECs) in small municipalities. The development of standardised multiresidue and multimatrix methods suitable for measuring a reliable number of CEC in environmental samples is crucial for monitoring infiltrating concentrations and for ensuring these systems' treatment capacity. The objective of this study is to develop and validate an analytical method for the simultaneous determination of CECs, including transformation products (TPs), with diverse physico-chemical properties, in environmental samples. The optimised method is based on sample clean-up and preconcentration by solid-phase extraction (SPE), followed by liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS). The method is able to detect and quantify 40 target CECs, including pharmaceuticals of different classes (analgesics, antibiotics, antihypertensives, lipid regulators, anticonvulsants, antidepressants, antiarrhythmics, beta-blockers, amongst others), hormones and lifestyle products with good reproducibility (variations below 23%), in different water matrices, and 28 CECs, in soil samples. Acceptable recoveries (65-120%) were obtained for most of the CECs in all the matrices. However in the soil samples, as complexity required a prior extraction treatment, the recovery of some analytes was affected, which reduced the number of target CECs. The achieved methodological quantification limits (0.05-5 ng/L and 0.04-1.1 ng/g levels for the water and the soil matrices, respectively) were reasonably low for most CECs. The proposed method was successfully applied to monitor CECs in a VF. The CECs detected at higher concentrations are some of the world's most widely used products (e.g. acetaminophen or caffeine and its main TP, paraxanthine). The results showed an almost 70% reduction in CEC concentrations during infiltration. The groundwater data indicated that the VF treatment operation did not affect the underlying aquifer (Cmax found in GW < 1 mu g/L).(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    A chromia-based sorbent for the enrichment of phosphotyrosine

    Alhendal, AbdullahRashad, MohammadHusain, AliMouffuok, Fouzi...
    7页
    查看更多>>摘要：Developing of new core@shell particles (CSPs) bearing metal oxides on their outer surfaces is of a great interest. Such hybrid systems have many benefits, i.e., low cost, operation simplicity, chemical stability and tunability along with simple recoverability and reusability that make them suitable as dispersive solid phase extraction (DSPE) sorbents for selecting/extracting different types of molecular structures. Accordingly, herein, novel chromia-based CSPs were successfully prepared and utilized as efficient DSPE for selective enrichment toward phosphotyrosine (pTyr). A modified version of Stober method was used to prepare highly dispersed core particles that were further coated with the chromium oxide. The outer shell surface morphology and thickness of SiO2 @Cr2O3-CSP system were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), whereas the surface functionalities were determined using X-ray photoelectron spectroscopy (XPS), FT-IR spectroscopy and zeta potential. The prepared chromia sorbent showed a significant improvement in extracting a probe-analyte (pTyr) compared to the results obtained by titania-based counterparts. As well to this, a noticeable stability of the SiO2 @Cr2O3-CSP sorbent was remarkably achieved which upon simple solvent-wash cycles, the studied sorbent can be regenerated/reused. Noticeably low-levels of LOD and LOQ (3.0 and 15 pg mL(-1) ) were attained with good linearity (R-2 of 0.9995), batch-to-batch reproducibility (RSD% <= 10) and run-to-run repeatability (RSD% <= 5.5).(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Metal organic frameworks as advance d adsorb ent materials for separation and analysis of complex samples

    Wang, BaichunYan, YinghuaDing, Chuan-Fan
    14页
    查看更多>>摘要：Sample pre-treatment is of great significance for study protein phosphorylation and glycosylation. Due to the low concentration and suppression of matrices, the direct detection of phosphoprotein and glycoprotein by mass spectrometry (MS) are still facing many challenges. The demand of efficient and specific enrichment of phosphoprotein and glycoprotein promotes the sample preparation methods based on metal-organic frameworks (MOFs). In this review, recent advances in MOFs-based samples pre-treatment, including the enrichment of protein, endogenous peptides, glycopeptides, phosphopeptides and glycans are summarized and discussed. In addition, the design and synthesis of different types of MOFs according to different enrichment mechanisms and principles are discussed. Furthermore, the potential problems of sample pre-treatment in proteomics is prospected.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Velvet-like carbon nitride as a solid-phase microextraction fiber coating for determination of polycyclic aromatic hydrocarbons by gas chromatography

    Wang, YanyanLian, LiliWang, XiyueYue, Boying...
    8页
    查看更多>>摘要：In this study, velvet-like carbon nitride (V-g-C3N4) was prepared from urea aqueous solutions by one-step thermal polycondensation. The V-g-C(3)N(4 & nbsp;)material was then characterized using a scanning electron microscope (SEM), X-ray diffractometer (XRD), Fourier transform infrared spectrophotometer (FT-IR), and nitrogen adsorption-desorption isotherms. The specific surface area of V-g-C3N4 (60.66 m(2)/g) was 1.8 times that of the carbon nitride (g-C3N4) prepared by the traditional method. V-g-C3N4 was modified on the surface of stainless-steel wire by a sol-gel technique to obtain a solid-phase microextraction (SPME) coating for the extraction of five polycyclic aromatic hydrocarbons (PAHs) from water samples. The chromatography signal of the PAHs extracted using the V-g-C3N4 coating was 1.5 times that when using a g-C3N4 coating, and 5-10 times that when using commercial PDMS. Under the optimized extraction conditions, the linear range of the method developed for the determination of five PAHs was 0.05-100 mu g/L, the limits of detection were 0.005-0.012 mu g/L, and the recoveries from actual water samples were 85.94-103.47%. Furthermore, the developed SPME device is remarkably durable and can be reused up to 160 times. (C)& nbsp;2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Simultaneous determination of 12 illicit drugs in human plasma by the PRiME clover-shaped nano-titania functionalized covalent organic frameworks pass-through cleanup procedure followed by ultra-performance liquid chromatography-tandem mass spectrometry

    Zhang, YunZhao, Yong-GangZhu, YanShi, Jia-Wei...
    7页
    查看更多>>摘要：A rapid and sensitive method based on PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure and ultra-performance liquid chromatography-tandem mass spec-trometry (UPLC-MS/MS) for the simultaneous determination of 12 illicit drugs in human plasma was de-veloped and validated. The clover-shaped nano-titania functionalized covalent organic frameworks (CSTF-COFs) has been evaluated in the PRiME pass-through cleanup procedure to remove blood phospholipids from plasma samples. Ion suppression effects can be dramatically reduced by CSTF-COFs based PRiME pass-through cleanup procedure. Under the optimal conditions, the results showed satisfactory recover-ies between 85.8% and 109%. Acceptable precision and accuracy were also obtained with RSD values less than 15.0% and RE values below 13.3%. The limits of detections (LODs) of 12 illicit drugs were in the range of 0.018-0.360 mu g/L. Furthermore, the PRiME CSTF-COFs cartridge could be conveniently regenerated and reused for 40-50 cycles. The proposed method was applied to real plasma samples from suspected drug abusers, which was proved to be reliable and robust for drug screening in clinical and forensic toxicology.(c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Reversed-phase capillary electrochromatography of pre-column derivatized mono- and oligosaccharides with three different ultraviolet absorbing tags

    Rajendiran, VaithilingamEl Rassi, Z.
    8页
    查看更多>>摘要：In this research report, an in house developed octadecyl monolithic (ODM) column has been exploited in the reversed-phase capillary electrochromatography (RP-CEC) of precolumn derivatized mono-and oligosaccharides with three different tagging agents, namely 1-naphthylamine (1-NA), 2-aminoanthracene (2-AA) and 3-amino-2,7-naphthalenedisulfonic acid (ANDSA). These three derivatizing agents, which differed in their charges, nonpolar characters and optical absorption properties, led to different RP-CEC elution patterns and UV detection signals. In fact, the limit of detection of the derivatized sugars were 50 mu M for the ANDSAand 1-NA-sugar derivatives and 35 mu M for the 2-AA-sugar derivatives due to the presence of three fused aromatic rings in 2-AA versus 2 fused rings in the 1-NA and ANDSA tags. Furthermore, while the longer ANDSA-oligosaccharides eluted later than the shorter ones and the ANDSAmonosaccharides, 1 -NA-and 2-AA-sugar derivatives necessitated the presence of borate ions at alkaline pH in the mobile phase to form in situ charged derivatives to facilitate their separation by RP-CEC, and the elution order was the reversal of that observed with the ANDSA-sugar derivatives; that is the mono-eluted later than the larger size oligosaccharides. In addition, plots of log tR vs. number of glucose residues (nGlc) for derivatized glucose and maltooligosaccharides yielded straight lines with slopes representing log 77 where 77 is the retention time modulus (i.e., ratio of retention time of two neighboring derivatives differing in one glucosyl residue). In the case of 1-NA and 2-AA derivatives, 77 was smaller than unity while it was greater than unity in the case of ANDSA-sugar derivatives because the elution occurred in the order of decreasing size of the homologous sugar derivatives in the former than in the later derivatives. The prepared ODM column was stable for more than a month of continuous use, a fact that allowed a good repeatability for intraday and interday analyzes.(C) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier

    Performance and selectivity of amphiphilic pillar[5]arene as stationary phase for capillary gas chromatography

    Sun, TaoZhang, WeiChen, RuonanLi, Wei...
    12页
    查看更多>>摘要：Pillar[n]arenes possess highly symmetrical and rigid pillar-shaped architecture with pi-electron rich cavity that afford their reliable host-guest recognition interactions towards matched guests. In this work, a novel amphiphilic pillar[5]arene (P5A-C10-2NH(2)) was designed, synthesized and employed as the stationary phase for capillary gas chromatography. To date, they have not been reported in the field of chromatography. The P5A-C10-2NH(2) capillary column (10 m x 0.25 mm i.d.) was prepared by static coating method. Its capillary column exhibited moderate polarity and column efficiency of 2265 plates/m determined by naphthalene at 120 degrees C. As evidenced, the P5A-C10-2NH(2) column achieved advantageous separation performance for a mixture of 24 analytes of diverse types and exhibited different chromatographic selectivity from two pillar[5]arene derivatives columns and commercial HP-35 column with 35%-phenyl-methylpolysiloxane. Moreover, the P5A-C10-2NH(2) column baseline resolved more than a dozen positional and cis-trans isomers. Furthermore, the separation mechanism of P5A-C10-2NH(2) column was discussed by quantum chemical calculations. In addition, the P5A-C10-2NH(2) column had high thermal stability and excellent separation repeatability 0.01-0.04% for run-to-run, 0.03-0.17% for day-to-day and 3.2-3.9% for column-to-column. The special amphiphilic structure and high resolution for various analytes reveal the good potential of pillararenes as a new class of stationary phases for chromatographic analyses. Moreover, the TPG column achieved improved thermal stability over the GIL column and excellent repeatability. (c) 2022 Elsevier B.V. All rights reserved.
      原文链接:
    • NSTL
    • Elsevier