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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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    The therapeutic effect of Xuanbai Chengqi Decoction on chronic obstructive pulmonary disease with excessive heat in the lung and fu-organs based on gut and lung microbiota as well as metabolic profiles

    Jiao, JiaoTang, QiWang, Tie-jieFan, Jin...
    13页
    查看更多>>摘要：As a prescription for treating lung inflammation and intestinal diseases, Xuanbai Chengqi Decoction (XBCQD) in clinical practice can effectively treat COPD with excessive heat in the lung and fu-organs, which is characterized by phlegm-heat accumulation in the lung and constipation. This study aims to find the potential biomarkers of COPD with excessive heat in the lung and fu-organs from two aspects of lung and intestine based on metabolomics and microbiota analysis, and to evaluate the efficacy of XBCQD as well as to explore the mechanism of drug function according the regulating effect of drugs on these markers. The HPLC-Q-TOF-MS/MS, 16SrDNA technology and multiple statistical methods were used to trace the process of disease and curative effect with XBCQD. Results showed that the onset and development of disease was associated with the imbalance of 41 differential metabolites in plasma, bronchoalveolar lavage fluid and feces and 82 bacteria at the levels of phylum, class, order, family and genus from lung and intestine, including Escherichia-Shigella. However, after treatment with XBCQD, 30 differential metabolites mainly involving in the metabolism of linoleic acid, taurine and hypotaurine metabolism, arachidonic acid metabolism, biosynthesis of primary bile acids, tryptophan metabolism, arginine and proline metabolism and 65 pulmonary and intestinal bacteria at all levels were reversed in the drug group. In addition, the results of the correlation analysis showed that specific microbiota from lung and intestine and reversed differential metabolites had a significant correlation, and they could affect each other in the course of disease occurrence and treatment. This study preliminarily confirmed that XBCQD can be used to treat COPD with excessive heat in the lung and fu-organs through lung-intestine simultaneous treatment. It also provided new strategies for the treatment of lung diseases or intestinal diseases, and new research ideas for the evaluation of drug efficacy.
      原文链接:
    • NSTL
    • Elsevier

    Simultaneous quantification of trimethoprim metabolites in pediatric plasma

    Tessman, Robert T.Nolte, WhitneyToren, PaulGibson, Kim...
    5页
    查看更多>>摘要：The dual agent antibiotic, trimethoprim/sulfamethoxazole (TMP-SMX), has been prescribed to treat or prevent infections for over 50 years. However, there are no published validated analytical methods for the measurement of TMP metabolites in humans. We developed methodology enabling reliable quantification of TMP and 5 me-tabolites in human plasma. Chromatographic separation was achieved in less than 8 min using a biphenyl col-umn. Analytes were detected in positive electrospray mode using a tandem Waters Xevo-TQ-XS mass spectrometer. Precision and accuracy values for all analytes were within 15% of nominal values during assay validation.
      原文链接:
    • NSTL
    • Elsevier

    Cyclophosphamide, hydroxycyclophosphamide and carboxyethyl phosphoramide mustard quantification with liquid chromatography mass spectrometry in a single run human plasma samples: A rapid and sensitive method development

    Kasudhan, Kripa ShankerPatial, AjayMehra, NancyAttri, Savita Verma...
    9页
    查看更多>>摘要：A novel method for simultaneous quantification of cyclophosphamide along with its two major metabolites namely 4-hydroxycyclophosphamide (HCy) and carboxyethyl phosphoramide mustard (CEPM) in a single sample run was demonstrated in the present study. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) instrument was used for analysis. Semicarbazide was used as a stabilizing agent for HCy whereas ifosfamide, hexamethyl phosphoramide mustard and deuterated CEPM were the internal standards for quantification of Cy, HCy and CEPM respectively. Chromatographic separation was achieved by Chromsystems C18 reverse-phase column (50 mm x 4.6 mm, particle size 3.2 mu m). The mobile phase was composed of eluent A (2 mM ammonium acetate in water with 2% formic acid) and eluent B (100 % acetonitrile). The flow rate was 1 ml/min. Linearity of the assay was assured in the range of 19.53 ng/ml to 10,000 ng/ml concentration in human plasma, which is adequate for pharmacokinetic studies of any dose Cy used clinically. The quality control(QC) accuracy was between 99.58% and 101.62%, 97.85% to 103.53% and 99.64% to 100.10% for Cy, HCy and CEPM respectively. Precision limits for QC samples were between 3.9% and 9.4%, 5.2% to 8.9% and 1.8% to 9.2% respectively. The analytical method was validated in ten leukaemia patients undergoing haploidentical hematopoietic cell transplantation.
      原文链接:
    • NSTL
    • Elsevier

    Development and validation of HPLC-DAD and LC-(ESI)/MS methods for the determination of sulfasalazine, mesalazine and hydrocortisone 21-ace- tate in tablets and rectal suppositories: In vitro and ex vivo permeability studies

    Tsamis, VasileiosTsanaktsidou, EleniKaravasili, ChristinaZacharis, Constantinos K....
    11页
    查看更多>>摘要：Controlled-release tablets and rectal suppositories of sulfasalazine (SLF) and hydrocortisone 21-acetate (HA) were prepared as recommended dosage forms for the treatment of acute episodes of ulcerative colitis, in patients who do not respond to monotherapy.A High-Performance Liquid Chromatography (HPLC) Diode-array method with a gradient elution mobile phase was developed to evaluate the production quality of both formulations (assay and dissolution profiles in gastric and intestinal fluids). Method's validation was carried out providing good linearity (r > 0.9995), precision (RSD < 1.53%), recovery (96.9% - 103.7%) and limits of detection (LODSLF = 12 ng/mL, LODHA = 15 ng/ mL). Experimental design and Plackett-Burman methodology was constructed to study the robustness of the analysis. In all composite substrates, a freezing lipid precipitation approach was used as purification step. The method was optimized by applying Central Composite design mode. The in-vitro/ex-vivo permeability studies of both formulations were evaluated by a Liquid ChromatographyElectron Spray Ionization Mass Spectrometry (LC-ESI/MS) +/- mode. The analysis of sulfamethazine (internal standard, SLM, m/z 279), HA (m/z 449, [M + HCOO]-), SLF (m/z 399) and its active metabolite mesalazine (MSL, m/z 154) was performed using a C18 column and gradient elution. The validation of the method met the requirements of the International Council for Harmonization (ICH) (r > 0.9997, RSD <= 4.62%, Recovery > 95%, LODSLF = 1.28 ng/mL, LODHA = 1.07 ng/mL, LODMSL = 3.16 ng/mL). Based on the results, important conclusions were drawn concerning the role of excipients and SLF metabolism.
      原文链接:
    • NSTL
    • Elsevier

    A sensitive HILIC-MS/MS method for quantification of theanine in rat plasma and tissues: Application to preclinical pharmacokinetic study

    Zhu, YanruWang, FengZhao, YunliYu, Miao...
    11页
    查看更多>>摘要：Adolescent depression is a significant public health problem, with the major depressive disorder having been the leading risk factor for suicide and death amongst children and adolescents. For treating depression, antidepressants are used with minimal clinical evidence data and uncertain efficacy in children. L-theanine has antidepression and other physiological functions. However, few reports are available on the pharmacokinetics of L-theanine, especially in children and adolescents. In this study, a rapid and sensitive hydrophilic interaction liquid chromatography-tandem mass spectrometry method was established and validated for the quantification of L-theanine in juvenile rat plasma and tissues. Chromatographic separation was conducted via an Agilent ZORBAX HILIC plus column in gradient elution mode. L-theanine and [2H5]-L-glutamic acid (internal standard) were determined under the multi-reaction monitoring mode transitions of m/z 175.0 -* 157.9 and m/z 153.0 -* 88.2 in positive ionisation mode, respectively, and completed methodology verification. In addition, 10 and 35 mg kg- 1 of L-theanine were given by intragastric administration to determine the brain and plasma pharmacokinetic characteristics in healthy and chronic unpredictable mild stress rats, respectively. The distribution of tissues and the limbic system were measured at the same time. The results showed that juvenile and diseased rats have higher absorption than adult rats, and age, dosage and health status could affect the process of L-theanine in vivo. L-theanine also has a high degree of tissue distribution. This study lays a foundation for the clinical treatment of depression in children and adolescents.
      原文链接:
    • NSTL
    • Elsevier

    Gold nanostructured membranes to concentrate low molecular weight thiols, a proof of concept study

    Berthou, MargauxPallotta, ArnaudBeurton, JordanChaigneau, Thomas...
    10页
    查看更多>>摘要：Thiols are very important molecules in the biomedical field involved for example in redox homeostasis. Their detection and quantification remain difficult due to their poor stability (oxidation) linked to their strong reactivity towards other thiols (by the formation of S-S bonds) or other interfering molecules in the medium. Cellulose membranes with immobilized gold nanoparticles (AuNP) were developed to capture and quantify thiols in simple and complex matrices. This device was first optimized and characterized in terms of nanostructuration and thiol adsorption. N-Acetylcysteine (NAC) and reduced glutathione (GSH), chosen as model molecules, were filtered through the device demonstrating a maximal adsorption capacity of 270 and 60 nmol respectively. In a second step, the adsorbed species were subjected to ligand exchange using a more reactive thiol, dithiothreitol. The results showed release rates of approximately 90% for NAC and GSH. Finally, the amount of endogenous GSH in rat plasma was determined without any pretreatment. For the first time to our knowledge, a nanostructured device for the capture, selective and sensitive quantification of thiols is proposed. This device is easy to handle and overcomes matrix effects. Moreover, the very large concentration factor induced by this technology will be a valuable asset to decrease the quantification limits of analytical methods.
      原文链接:
    • NSTL
    • Elsevier

    Comprehensive site- and structure-specific characterization of N-glycosylation in model plant Arabidopsis using mass-spectrometry-based N-glycoproteomics

    Qin, ShanshanQin, SuidengTian, Zhixin
    6页
    查看更多>>摘要：The N-glycosylation is an important bioprocess in plant. Monosaccharide composition-level characterization at the intact N-glycopeptides has been extensively reported, yet structure-specific study to resolve multiple sequence structures of a single composition is still lacking. Here, we present a comprehensive structure-specific identification of intact N-glycopeptides of Arabidopsis with both HILIC and RAX enrichment, as well as GPSeeker and pGlyco database search. With target-decoy searches and spectrum-level FDR <= 1%, 5,687 N-glycopeptides from 3,713 N-glycosites of 3,140 N-glycoproteins were identified, which represents the currently most comprohensive profilling to our best knowledge. Wtih the experimental evidence support of structure-diagnostic fragment ions, 81 glycan structures from 54 glcan compostions were unambiguouly distinguished. The comprehensive experimental site- and structure-specific N-glycosylation data reported in this study will serve as a fundamental valuable reference for the coming functional studies of this widely adopted model organism of plant.
      原文链接:
    • NSTL
    • Elsevier

    Effect of the ethyl acetate extract of Sophora flavescens Aiton on diabetic retinopathy based on untargeted retinal metabolomics

    Wang, ShumeiLiu, YiChen, LeiLuo, Yun...
    12页
    查看更多>>摘要：Diabetic retinopathy (DR) is the most common microvascular complication of diabetes and a leading cause of vision impairment and blindness, which lacks effective diagnostic measures and therapeutic options. Sophora flavescens Aiton or "Kushen" is a traditional Chinese medicine used since ancient times, either alone or in combination, to clear heat, dampness, and tearing, and to treat ocular diseases and improve eyesight. Additionally, the flavonoids of Sophora flavescens Aiton extracted using ethyl acetate (EtOAc) (SFE) is effective in managing diabetes and diabetic vascular complications. In this study, we explored the pharmacodynamic effects and material basis of action of SFE on DR for the first time and elucidated the mechanism based on untargeted retinal metabolomics. Results from the pharmacodynamic studies showed that SFE could reduce blood glucose levels in rats, regulate serum lipopolysaccharide, tauroursodeoxycholic acid, and trimethylamine oxide levels, and significantly improve the structure of retina in rats with DR. Moreover, SFE could protect the blood-retinal barrier, reduce angiogenesis and capillary formation, and inhibit retinal nerve cell apoptosis. A total of 13 compounds were identified in the aqueous humor and retina, which were dihydroflavonoid, isoflavonoid, pterostane flavonoid, chalcone, and dihydroflavonol derivatives. In addition, 39 differential metabolites were screened based on retinal metabolomics data and 23 were found to be affected by SFE, indicating its anti-DR effect by regulating the synthetic metabolic pathways, including lactose, bile acid, glycerophospholipid, arginine, purine, and pyrimidine metabolism pathways. Collectively, our findings elucidated the effects, material basis, and treatment mechanism of SFE on DR systematically and could lay the foundation for promoting the clinical application of Sophora flavescens Aiton.
      原文链接:
    • NSTL
    • Elsevier