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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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    Accumulation of zoledronic acid in rabbit intervertebral discs

    Christophoridis, ChristophorosKouroumalis, AnastasiosKletsas, Dimitris
    9页
    查看更多>>摘要：Low back pain is a major chronic musculoskeletal disorder, caused mainly due the degeneration of the inter vertebral discs (IVDs). Bisphosphonates (BPs), like zoledronic acid (ZOL), are used in osteoporosis management; however, their accumulation in the IVDs and their physiological role has not been addressed so far. To this end, an SPE-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) analytical method, using on cartridge derivatization, has been developed and validated. The analytical method presented excellent linearity (R-2 > 0.992), high recoveries (67.8-82.6%), increased repeatability (0.5-9.9%) and low LOD values (21 ng g(-1) in the case of IVDs) in all matrices studied. The injection of ZOL in a rabbit animal model resulted in rapid accumulation in blood plasma and the skin, followed by quick clearance. On the other hand, no ZOL was detected in nucleus pulposus, the core of the IVD, while in the peripheral annulus fibrosus a lower and delayed accumulation, as well as dispersal was found. These variations are most probably due to the avascular nature of IVD, allowing only the diffusion of small molecules in and out of the tissue, and/or to the unique physicochemical environment of IVDs. Finally, ZOL, at the concentrations found, did not affect cells' viability or the increase of reactive oxygen species (ROS).
      原文链接:
    • NSTL
    • Elsevier

    Potential efficacious materials investigation of Yi-Yi Mixture based on Metabolome-oriented network pharmacology strategy

    Gong, Guan-WenTang, Wei-HongZhou, ZhuoJiang, Yan-Wen...
    16页
    查看更多>>摘要：Yi-Yi Mixture, an efficient Chinese medicine preparation composed of four herbal medicines, has been used in clinical practice in China for the treatment of acute pancreatitis over twenty years. However, its functional materials against acute pancreatitis remains unclear, which is a huge obstacle for quality control. In this study, a metabolome-oriented network pharmacology strategy was proposed to clarify its potential substances and further screen out quality markers. Firstly, an Ultra-High performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method was utilized to profile the chemical constituents in Yi-Yi Mixture. Secondly, metabolic exposure of chemical constituents as well as their global metabolites produced in biological systems were profiled and defined as metabolome of Yi-Yi Mixture. Then, the metabolome targets were predicted based on network analysis. As a result, a total of 66 chemical components were characterized, including 6 stilbenes, 21 anthraquinones, 7 phenols, 13 neolignans, 3 naphthalenes and 16 other types. Moreover, metabolic profiles of YYM (32 prototypes and 37 metabolites) were analyzed in rat bio-samples. Among them, resveratrol, emodin, chrysophanol, rhein and their derivatives were detected in multiple tissues/organs, revealing their potential as key pharmacodynamic substances. These were further confirmed by metabolomeoriented network analysis and molecular docking techniques. This is the first comprehensive investigation on chemical and metabolic profiles of Yi-Yi Mixture, and the results provided scientific foundation for further research on quality control and clinical-safe medication administration.
      原文链接:
    • NSTL
    • Elsevier

    Application of Fe3O4@TbBd nanobeads in microextraction by packed sorbent (MEPS) for determination of BTEXs biomarkers by HPLC-UV in urine samples

    Kurd, NematullahBahrami, AbdulrahmanAfkhami, AbbasShahna, Farshid Ghorbani...
    10页
    查看更多>>摘要：A relatively new adsorbent based on covalent organic frameworks (COFs) was employed for the first time to extract and determine Trans, trans-muconic acid (tt-MA), Mandelic acid (MA), Hippuric acid (HA), and 3-Meth-ylhippuric acid (m-MHA) in urine. For this purpose, microextraction was performed using the packed sorbent (MEPS) method. Following the extraction process, the prepared samples were specified via the high-performance liquid chromatography-ultraviolet detector system. The precipitation polymerization was applied to synthesize the Fe3O4@TbBd nanobeads, and the morphological and dimensional structures of the products were specified with FE-SEM images. Some key variables affecting the extraction efficiency (i.e., sample volume, elution volume, condition and washing solvents, type and volume of elution solvent, extraction cycles, temperature, and pH of the sample solution) were investigated. In ideal conditions, the limit of detection (LOD) was obtained from 0.02 mu g/ml for tt-MA to 0.5 mu g/ml for MA. Calibration curves (at five-point) were plotted in the range 0.05-5 mu g/ml for tt-MA to 1-300 mu g/ml for MA (R2 > 0.98). Moreover, intra-and inter-day precision values were 3.1-5.5 and 4.6-9.8%, respectively. The developed method was successfully employed to determine four analytes in three concentrations (low, medium, and high QCs). The results showed a satisfactory recovery (70-87%). COF-MEPS technique is a rapid, easy, user-friendly, and environment-friendly method for separating the minimum values of all BTEXs chief biomarkers from urine samples without using complicated processes and only with one adsorbent. Also, it can be a good alternative for biomonitoring the workers exposed to BTEX compounds in occupational and environmental access.
      原文链接:
    • NSTL
    • Elsevier

    Fishing for lipid lactones using selective reaction and characteristic fragmentation pattern

    Smith, Elana A. SlutskyKhatib, SolimanSzuchman-Sapir, Andrea
    10页
    查看更多>>摘要：Extensive research has been invested in developing sensitive methods to identify lipid mediators (LMs) from multiple biological matrices. Previous studies point to the existence of a potential family of lactone-containing metabolites generated from eicosanoid families, isoprostanes, and prostanoid-like compounds that may func-tion as LMs. However, targeted lipidomic studies do not routinely include lactone-containing lipids due to their low ionizability and instability under some common sample preparation conditions. Thus, the discovery of lactone-containing LM is limited. Herein we describe a method for selective identification of lipid lactones from within biological matrices. This method is based on a selective reaction of lactones with 1-(3-aminopropyl)imidazole, followed by cation ex-change solid phase extraction and the identification of characteristic fragmentation patterns unique to reaction products of lactones in LC/MS/MS. NMR and LC/MS results indicated that saturated and unsaturated aliphatic gamma and 8 lactone model compounds mixed with human serum were successfully detected. MS/MS analyses of the reaction products revealed a unique pattern for the lactones, resulting from common neutral losses and frag-mentation. When applied to esters and free fatty acids, some reaction products were observed. However, these reaction products' MS/MS fragmentation did not match the specific fragmentation of the lactones' reaction products. Confirming that lactones can be detected in a highly selective manner from within complex biological matrices when using the presented method. Thus, the presented method can selectively analyze lactones and may further complement existing lipidomic approaches to discover new LMs.
      原文链接:
    • NSTL
    • Elsevier

    Development and validation of a direct HPLC method for the determination of salivary glutathione disulphide using a core shell column and post column derivatization with o-phthalaldehyde

    Tsiasioti, ApostoliaGeorgiadou, EiriniZacharis, Constantinos K.Tzanavaras, Paraskevas D....
    6页
    查看更多>>摘要：Glutathione disulfide (GSSG) has been monitored in human saliva samples by an optimized and validated method that is based on liquid chromatography coupled to on-line post column derivatization. The analyte was separated from the sample matrix using a 100% aqueous mobile phase through a core-shell reversed phase column. Following optimization of the reaction using Box-Behnken experimental design and validation, GSSG was quantified accurately and selectively in the range of 100-2000 nmol L-1 with a LOD of 20 nmol L-1. GSSG was quantified in 15 out of 20 human saliva samples (75%) with a mean value of 860 nmol L-1 (150-4600 nmol L-1). Blocking of reduced Glutathione with N-ethylmaleimide ensured stability of the samples for at least 72 h at all temperatures examined.
      原文链接:
    • NSTL
    • Elsevier

    Simultaneous determination of almonertinib and its active metabolite HAS-719 in human plasma by LC-MS/MS: Evaluation of pharmacokinetic interactions

    Liu, LuYang, LeLi, WeiChen, Xiaoyan...
    7页
    查看更多>>摘要：The combination of two or more drugs in a clinical setting has an impact in pharmacokinetics, drug efficacy and safety, and the study of these interactions has attracted considerable attention over the last years. In the present study, we have developed a LC-MS/MS method for the sensitive and reliable quantification of almonertinib and its active metabolite HAS-719. Further, we investigated the effects of their pharmacokinetics in humans by using modulators of CYP3A, an almonertinib-metabolizing enzyme. Analytes were extracted from plasma samples via acetonitrile-induced protein precipitation and separated on a BEH C18 column using ammonium acetate with formic acid and acetonitrile as the mobile phase. Electrospray ionization in positive ion mode and multiple reaction monitoring were used to monitor the ion transitions at m/z 526-* 411 and 512-* 423. Validation was performed in the range 0.500 to 500 ng/mL for both the analytes of interest according to the guidelines of the U. S. Food and Drug Administration and European Medicines Agency, sufficient to account for variations in plasma concentrations caused by the presence of CYP3A modulators. The selectivity, precision, accuracy, recovery and matrix effect of this method were all within acceptable limits of bioanalytics. The interference of CYP3A modulators itraconazole and rifampicin with the analytes, and the mutual interference between the analytes were also investigated producing acceptable results. The method herein described was successfully applied for the pharmacokinetics evaluation of almonertinib in healthy subjects exposed to a single dose of almonertinib (110 mg), with or without itraconazole or rifampicin.
      原文链接:
    • NSTL
    • Elsevier

    Serum metabolomic research of the anti-pulmonary fibrosis effects of Shuangshen Pingfei Formula on bleomycin-induced pulmonary fibrosis rats

    Chen, YeqingLi, LinlingWang, WenlongSun, Yunpeng...
    9页
    查看更多>>摘要：Our previous studies showed that Shuangshen Pingfei Formula (SSPF) exhibited anti-fibrosis effect, but its biochemical changes at the metabolic level remain unclear. In this study, an integrative approach of gas chromatography-mass spectrometry (GC-MS) and ultra performance liquid chromatography-Q Exactive-mass spectrometry (UPLC-QE-MS)-based non-targeted metabolomics and multivariate statistical analysis was employed to explore the metabolic changes of serum samples from different stages of bleomycin-induced pulmonary fibrosis (PF) rats (PFRs: M7, M14, M21 and M28) treated with SSPF extracts. Potential biomarkers for PF were screened. Benzenebutanoic acid, pyroglutamic acid, cholic acid, 1-monopalmitin, succinic acid and palmitoleic acid may be potential biomarkers of the early inflammation stage of PF (M7-M14). 3,4-dimethylbenzoic acid, glutamic acid, glycine, proline, serine, taurine, etc. may be potential biomarkers for the advanced pulmonary fibrosis stage (M21-M28) of PF. The disturbance was mainly related to the disorder of lipid, amino acid metabolism. After SSPF treatment, the disorder was regulated and 67 metabolites were restored to a certain extent. Serine, proline, glutamine, 4-guanidinobutyric acid, phosphatidylethanolamine, lecithin and 9,10-epoxyoctadecene acids may be useful as biomarkers of the anti-fibrosis effect of SSPF.
      原文链接:
    • NSTL
    • Elsevier