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Journal of chromatography
Elsevier
Journal of chromatography

Elsevier

1570-0232

Journal of chromatography/Journal Journal of chromatography
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    High sensitivity acidic N-glycan profiling with MS-enhancing derivatization and mixed mode chromatography

    Liu, XiaoxiaoWang, QiLauber, Matthew A.
    7页
    查看更多>>摘要：Acidic N-linked glycan content is often associated with a protein drug's stability, efficacy and immune response. It has often been a challenge to analyze these types of glycans, including those that are differentiated by the incorporation of N-acetyl (NANA) and N-glycolyl neuraminic acid (NGNA) residues. In this study, a strategy for rapid N-glycan profiling by mixed mode chromatography is proposed as a complement to established HILIC methodologies. Hybrid silica chromatographic surfaces are used to improve recoveries during a column's initial use and to eliminate the need for column conditioning. In addition, the loss of labeled acidic glycans, especially phosphorylated glycan species, during SPE purification is addressed through the use of a citrate containing eluent. Yields for both singly and doubly phosphorylated glycan species are markedly improved. Combined with a mixed mode anion exchange reversed phase separation, these advances afford a class separation of glycans derivatized with labels designed to enhance positive ion mode MS detection. These labeled glycan species are separated according to their charge and with an added level of resolution imparted by the reversed phase retention mechanism. The separation technique itself can be accomplished with a low ionic strength gradient running from 0 to 22 mM ammonium formate such that high sensitivity detection can be achieved by both fluorescence and mass spectrometry. Using analytical scale chromatography, features in an N-glycan profile were easily interrogated to well below a 0.1% relative abundance. As such, it became possible to characterize Nglycans from recombinant beta glucuronidase and to quickly identify a number of unique phosphorylated glycan species.
      原文链接:
    • NSTL
    • Elsevier

    Studies on the mechanism of Panax Ginseng in the treatment of deficiency of vital energy dementia rats based on urine metabolomics

    Huang, YuLiu, ZhiqiangLiu, ShuSong, Fengrui...
    9页
    查看更多>>摘要：Panax Ginseng (PG) has been used to strengthen memory and physique for thousands of years, because its main components ginsenosides (GS) and ginseng polysaccharides (GP) play a major role, but its mechanism is not clear. In this study, a rat model of dementia with vital energy deficiency (DED) was established through intraperitoneal injection with D-galactose and AlCl3 and combined with exhaustive swimming. Pharmacological studies and the urine metabolomics based on ultra-high-performance liquid chromatography-quadrupole timeof-flight mass spectrometry (UPLC-Q-TOF-MS) were employed for evaluation the efficacy of PG and exploring this treatment mechanism. Through urine metabolic profiling, it can be seen that DED rats after PG administration are close to normal group (NG) rats, and PG can regulate the in vivo status of DED rats which tend to NG. The results of behavioral, biochemical indicators and immunohistochemistry further verified the above results, and the mechanism of action of each component is refined. Ultimately, we believe that the mechanism of PG in the treatment of DED is that ginsenosides (GS) intervenes in phenylalanine tryptophan and tyrosine metabolism, stimulates dopamine production, inhibits A beta deposition and neuroinflammation; and that ginseng polysaccharides (GP) provides energy to strengthen the TCA cycle and improve immune capacity.
      原文链接:
    • NSTL
    • Elsevier

    Thermosensitive molecularly imprinted polymer coupled with HPLC for selective enrichment and determination of matrine in traditional Chinese medicine

    Xu, XinyaXue, WeimingWang, YichenSong, Xiaoping...
    11页
    查看更多>>摘要：In this study, a temperature-sensitive molecularly imprinted polymer was prepared by using the bifunctional monomer with the critical phase transition characteristics. Infrared spectrometry, scanning electron microscopy, and specific surface area testing were used to characterize the polymers. Then, the recognizing properties of the polymers were studied. Based on the prepared smart polymers, an SPE-HPLC analytical method for the determination of quinolizidine alkaloids in the extracts of Sophora flavescens was established and verified. Finally, the smart polymers were applied to the enrichment of quinolizidine alkaloids in plant extracts. By changing the temperature and solvents of the solid phase extraction conditions, the extraction process can increase the concentration of quinolizidine alkaloids by 4.3 to 5.2 folds. The extraction process has mild conditions and less time consumption, avoiding the use of a large number of toxic reagents, which indicate that the extraction process are more efficient and environmentally friendly.
      原文链接:
    • NSTL
    • Elsevier

    Quantitative structure retention relationship (QSRR) modelling for Analytes' retention prediction in LC-HRMS by applying different Machine Learning algorithms and evaluating their performance

    Liapikos, T.Zisi, C.Kodra, D.Kademoglou, K....
    10页
    查看更多>>摘要：In metabolomics, retention prediction methods have been developed based on the structural and physicochemical characteristics of analytes. Such methods employ regression models, harnessing machine learning algorithms mapping experimentally derived retention time (tR) analytes with various structural and physicochemical descriptors, known as Quantitative Structure Retention Relationships (QSRR) models. In the present study, QSRR models have been developed by applying four Machine Learning regression algorithms, i.e. Bayesian Ridge Regression (BRidgeR), Extreme Gradient Boosting Regression (XGBR) and Support Vector Regression (SVR) using both linear and non-linear kernels, all tested and compared for their retention prediction ability on experimentally derived and on publicly available chromatographic data, using Molecular Descriptors to describe the physical, chemical or structural properties of molecules. Various configurations of the available datasets, in terms of the highly-correlated features levels (defined as the maximum absolute value of the Pearson's correlation coefficient calculated between any pair of features) they contained, were analyzed in parallel. This is the first study, to the best of our knowledge, of the effect of collinearity on the performance of QSRR predictive models. In the vast majority of cases studied there was no statistically significant difference in the performance of the generated QSRR predictive models among the specified dataset configurations, indicative of the ability of the selected regression algorithms to effectively handle collinearity. In terms of the individual performance of the selected regression algorithms, no pattern was found where one algorithm (or class of algorithms) stood out significantly relative to the others among the study datasets.
      原文链接:
    • NSTL
    • Elsevier

    Quality analysis of Euryales Semen from different origins and varieties based on untargeted metabolomics

    Bao, KeJing, ZonghuiWang, QianHuang, Zhiheng...
    8页
    查看更多>>摘要：Euryales Semen (ES) is sought-after for thousand years due to its multiple properties, mainly from the two cultivars (i.e. South Gordon Euryale (SE) and North Gordon Euryale (wild type, WT)). Currently, no effective way was established to recognize the two valuable and analogous kernels. We found high analogies of macroscopical traits and discovered WT seed was affected by ambient temperature, showing ostensible significant relationships with latitude and sea-level pressure. LC-MS based untargeted metabolomics helped us identified 177 putative metabolites. Pathway analysis revealed the underlying and vital roles of flavonoids during seeds development. Our results strongly suggested a strong level of similarity of WT from various regions on the strength of metabolic data. A multivariable model containing 51 chemical markers satisfactorily categorized WT and SE. This study obtained could be used to guide the varietal discrimination of ES.
      原文链接:
    • NSTL
    • Elsevier

    Application of novel mixed mode chromatography (MMC) resins having a hydrophobic modified polyallylamine ligand for monoclonal antibody purification

    Aoyama, ShigeyukiMatsumoto, YoshihiroMori, ChigusaSota, Kojiro...
    10页
    查看更多>>摘要：Polyallylamine (PAA) has been utilized as a salt tolerant anion exchange chromatography ligand in downstream processing of biopharmaceuticals. We have developed novel MMC resins based on PAA polymer ligand partially modified with hydrophobic butyl or phenyl group. The resulting hydrophobic modified PAA ligand reduced HCP level to 12% (21-23 ppm) under 6 mS/cm in a flow-through polishing step of mAb, while not modified PAA ligand showed only 79% (145 ppm). We also found that structure of hydrophobic groups in the ligand mainly influenced on mAb yield. That is 25% increase of phenyl group modification ratio reduces mAb yield from 95% to 90%. On the other hand, modification with butyl group kept mAb yield more than 95%. The optimized ligand structure displayed a wide operational conductivity range. Extended purification studies of mAb using the MMC resin in the flow-through polishing step were carried out under optimized pH and conductivity condition as determined in a DOE study. The study revealed that the MMC resin was effective for developing one-step flow-through polishing workflow for mAb purification. In addition, the MMC flow-through polishing step could be directly coupled with a specified CEX chromatography step to efficiently remove mAb aggregates from 2.3% to <1.0% to achieve a biopharmaceutical-grade quality and a high yield of mAb (>93%) with a high loading ca-pacity around 1000 mg/mL-resin. This new MMC resin will be useful in future mAb manufacturing platforms comprising of a robust and cost-effective flow-through polishing step.
      原文链接:
    • NSTL
    • Elsevier

    An ultrasensitive colloidal gold immunosensor to simultaneously detect 12 beta (2)-adrenergic agonists

    Xu, XiaoxinXu, XinxinSun, LiWu, Aihong...
    9页
    查看更多>>摘要：In this study, we first prepared a selective monoclonal antibody against 12 beta (2)-adrenergic agonists (Salbutamol, Clenbuterol, Brombuterol, Clenpenterol, Mabuterol, Carbuterol, Cimbuterol, Mapenterol, Pirbuterol, Terbutaline, Cimaterol, and Clenproperol). Then three haptens were designed and derived, among which, hapten(S3) used the amino group of the salbutamol analog to derive a carboxyl group containing a spacer, which is unique to this study. The half-maximal inhibitory concentration (IC50) values were 0.35 ng/mL (Salbutamol), 0.42 ng/mL (Clenbuterol), 0.78 ng/mL (Brombuterol), 0.88 ng/mL (Clenpenterol), 1.34 ng/mL (Mabuterol), 1.38 ng/mL (Carbuterol), 1.71 ng/mL (Cimbuterol), 2.24 ng/mL (Mapenterol), 2.25 ng/mL (Pirbuterol), 2.27 ng/mL (Terbutaline), 3.49 ng/mL (Cimaterol), and 4.89 ng/mL (Clenproperol). We further developed a monoclonal antibody-based colloidal gold immunochromatographic test strip for screening and detecting 12 beta (2)-adrenergic agonists in swine urine and lamb samples. The immunochromatographic method developed in this study is a suitable tool for the on-site rapid detection and screening of beta (2)-adrenergic agonists in swine urine and lamb samples.
      原文链接:
    • NSTL
    • Elsevier

    Comparison of chemometric assisted targeted and untargeted approaches for the prediction of radical scavenging activity of ylang-ylang essential oils

    Lebanov, LeoPaull, Brett
    10页
    查看更多>>摘要：Essential oils have been used for centuries for their preservative properties. An example is ylang-ylang Cananga odorata [Lam.] Hook. f. & Thomson essential oil, which exists in four different distillation grades, where the fraction with the longest distillation time has the highest radical scavenging activity (RSA). Gas chromatography mass spectrometry (GC-MS) followed by multivariate statistical analysis is a powerful approach for determination of RSA. Herein the performance of such multivariate statistical analysis using three data sets derived from gas chromatography mass spectrometry (GC-MS) analysis, is compared to that achieved using two direct and fast spectroscopic techniques, for the prediction of RSA using partial least squares (PLS) regression analysis. The three GC-MS data sets were, 'full chemical composition', 'total chromatogram average mass spectra (TCAMS)' and 'segment average mass spectra (SAMS)', whilst two spectroscopic techniques, namely attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and Raman spectroscopy, provided the spectroscopic data sets for comparison. PLS models created using ATR-FTIR and 'full chemical composition' data sets provided the lowest relative error of prediction (REP) and mean error of prediction (MEP) in validation, whilst in independent test sets, the PLS models created using ATR-FTIR and SAMS data sets delivered the lowest REP and MEP. The three GC-MS derived data sets were further compared for value in determination of compounds contributing to the RSA. PLS regression analysis of the full chemical composition data set revealed that germacrene D and (E,E)-alpha-farnesene were the major contributors to the RSA, whilst average mass spectrum based data sets, TCAMS and SAMS, also highlighted eugenol as another contributor to the RSA.
      原文链接:
    • NSTL
    • Elsevier

    A rapid HPLC-MS/MS method for the simultaneous determination of luteolin, resveratrol and their metabolites in rat plasma and its application to pharmacokinetic interaction studies

    Wu, WenyingLi, KexinZhao, ChenRan, Xiaohua...
    9页
    查看更多>>摘要：Both luteolin (LUT) and resveratrol (RES) are natural polyphenols that exert therapeutic effects on liver injuries. Extensive glucuronidation by uridine diphosphate-glucuronosyltransferases 1As (UGT1As) results in poor bioavailability of LUT, which limits its clinical application. As an inhibitor of UGT1A1 and UGT1A9, RES may affect the bioavailability of LUT. The purpose of this study was to develop and validate an HPLC-MS/MS method for the simultaneous determination of LUT, luteolin-3'-O-glucuronide (LUT-3'-G), RES and resveratrol-3-O-glucuronide (RES-3-G) in rat plasma to investigate the effects of RES on the bioavailability and metabolism of LUT after coadministration. The samples were extracted by protein precipitation with methanol using daidzein and naringenin as the internal standards. Separation was achieved on an XBridgeTM C18 column by isocratic elution using 88% methanol-12% water with 2 mM ammonium acetate and 0.01% formic acid. Multiple reaction monitoring mode with a negative electrospray ionization interface was used for quantification of the analytes. The calibration curves were linear over the concentration ranges of 1-1000 (r > 0.995), 2-2000 (r > 0.999), 5-5000 (r > 0.998) and 10-40000 ng/mL (r > 0.996) for LUT, LUT-3'-G, RES and RES-3-G, respectively. The method was fully validated in terms of accuracy, precision, matrix effect, recovery and stability. The validated data met the acceptance criteria in FDA guidelines. The method was successfully applied in a pharmacokinetic interaction study of LUT and RES. The results indicated that RES had a significant effect on the enhanced bioavailability of LUT by reducing the major glucuronidation metabolite in rats, which provides a reference for the combination of LUT and RES in liver diseases.
      原文链接:
    • NSTL
    • Elsevier

    Determination of terbinafine in healthy Chinese human plasma using a simple and fast LC-MS/MS method and its application to a bioequivalence study

    Yang, CanLiu, LuyaoSheng, MangFu, Rong...
    8页
    查看更多>>摘要：A rapid, simple, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was validated for the determination of terbinafine concentrations in the plasma of healthy Chinese subjects. Terbinafine-d7 was used as the internal standard (IS), and the acetonitrile protein precipitation method was selected. The processed samples were chromatographically separated with a C18 column. The mobile phases were 0.1% formic acid (FA) in water (A), and methanol (B), respectively, and the gradient elution program was used with a flow rate of 0.8 mL/min. Quantification was achieved by positive electrospray ionization containing multiple reaction monitoring (MRM) transitions of m/z 292.5-* 141.1 for terbinafine and m/z 299.5-* 148.1 for IS. The calibration curve range was 2.00-1200 ng/mL; the intra-and inter-batch precision (coefficient of variation, %CV) was <8.2%, with the accuracy deviation (relative error, %RE) of-6.5% to 10.2%. The selectivity, sensitivity, extraction recovery, matrix effect, dilution reliability, carryover, and stability were within the acceptable range. This method was successfully applied to a bioequivalence study that orally administered 125 mg of terbinafine hydrochloride tablets in 84 healthy Chinese subjects.
      原文链接:
    • NSTL
    • Elsevier