首页期刊导航|Journal of chromatography
期刊信息/Journal information
Journal of chromatography
Elsevier
Journal of chromatography

Elsevier

1570-0232

Journal of chromatography/Journal Journal of chromatography
正式出版
收录年代

    Preparation of molecularly imprinted foam for selective extraction of toxic monocrotaline from herbs

    He, NaLi, XuanLuo, ZhiminWang, Lu...
    8页
    查看更多>>摘要：Monocrotaline (MCT), derived from most flowering plants, showed significant hepatotoxicity and carcinoge-nicity. Humans are easily exposed to MCT by eating traditional herbs or contaminated foods, posing a huge threat to human health. In order to selectively and conveniently separate and enrich MCT from these complex samples, we fabricated three-dimensional porous and homogeneous molecularly imprinted polymer foams (MIPFs) by using considerably inexpensive polyurethane foam (PU) as the carrier. The morphology, stability, adsorption properties and extraction parameters of MIPFs were investigated. The results indicated that an imprinted layer was coated on the surface of the carrier; the stability of MIPFs was excellent; In addition to hydrogen bonding and spatial complementarity, the electrostatic interactions were crucial for the recognition between MCT and MIPFs; MIPFs exhibited high adsorption capacity of 22.78 mg g(-1), fast mass transfer rate, and satisfactory selectivity for MCT. Subsequently, MIPFs were applied as the solid phase extraction (SPE) absorbents and combined with high performance liquid chromatography (HPLC) to enrich and detect MCT in herbal plants. The results showed that MCT could be efficiently enriched, and the impurities could be dramatically reduced. MIPFs hold great potential for selective separation and detection of MCT in complex matrices, such as traditional Chinese medicine samples and food samples.
      原文链接:
    • NSTL
    • Elsevier

    Determination of free and encapsulated cytarabine and daunorubicin in rat plasma after intravenous administration of liposomal formulation using ultra-high performance liquid chromatography tandem mass spectrometry

    Li, ShaZeng, ShiWei, Bo-pingWu, Qiang...
    9页
    查看更多>>摘要：Liposome encapsulating cytarabine (CYT) and daunorubicin (DNR) is applied for treating Acute Myeloid Leukemia (AML) patients. To evaluate and compare relationship between the pharmacokinetics of free drug (drug which is not entrapped in liposomes) and liposome-encapsulated drug and the toxicity/efficacy, it is crucial to have trustworthy methods for separating the free and the encapsulated of the drug. In this study, methods were developed and validated to isolate and measure the free DNR/CYT (F-DNR/CYT), the encapsulated DNR/CYT (EDNR/CYT) and the total DNR/CYT (T-DNR/CYT) in rat plasma. The methods involved solid-phase extraction (SPE) using reverse adsorbents for separating the F-DNR and E-DNR, SPE using cation exchange adsorbents for separating the E-CYT, ultrafiltration for isolating the F-CYT and protein precipitation (PPT) for releasing the TDNR and T-CYT totally from the liposomal forms. The analytes were subsequently quantified on ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) individually with multiple reaction monitoring (MRM) mode using positive electrospray ionization (ESI). The calibration curves showed good linear relationships over the concentration range of 0.22-44 mu g/mL for E-DNR and T-DNR, 2-1000 ng/mL for FDNR, 0.5-100 mu g/mL for E-CYT and T-CYT, 4-2000 ng/mL for F-CYT respectively. For all the analytes, the within-and between-run precisions were less than13.6% and the accuracies (in terms of RE%) were within-12.5%. Besides, extraction recovery, matrix effect, dilution integrity and stability were also assessed. The methods were successfully applied to investigate the pharmacokinetics in Sprague-Dawley rats following i.v. administration liposomal formulation.
      原文链接:
    • NSTL
    • Elsevier

    High performance Reversed-Phase Thin-Layer Chromatography-Desorption electrospray ionisation - time of flight high resolution mass spectrometric detection and imaging (HPTLC/DESI/ToFMS) of phytoecdysteroids

    Claude, EmmanuelleLafont, RenePlumb, Robert S.Wilson, Ian D....
    7页
    查看更多>>摘要：Reversed-phase high performance thin-layer chromatography (RP-HPTLC) on C18 bonded silica gel was combined with desorption electrospray ionization (DESI) and high resolution time of flight mass spectrometry (HRToFMS) to detect, characterize and image (MSI) phytoecdysteroids (plant-derived insect moulting hormones) in ethanolic extracts of members of the Silene plant family. As seen previously for silica gel, DESI provided a simple and convenient method for recovering polar polyhydoxysteroids from RP-HPTLC plates for the purposes of both the MS and MSI of extracts obtained from three species of the Silene family (Silene otites, S. nutans and S. viridiflora). Using RP-HPTLC/DESI/MSI/HRToFMS a number of ecdysteroids, including 20-hydroxyecdysone, polypodine-B, 2-deoxy-20-hydroxyecdysone and 2-deoxyecdysone were identified in these extracts. Differences were noted in the mass spectra obtained depending upon both the stationary phase on which they were separated, and the temperatures used in the heated transfer line used for introduction into the ion source. Ecdysteroids detected after chromatography on C18 bonded silica showed increased fragmentation due to water loss compared to those imaged from silica. In addition, the benefits of the additional resolution provided by 2-dimensional TLC for increasing spectral quality compared to a 1-dimensional separation are demonstrated.
      原文链接:
    • NSTL
    • Elsevier

    Integrated approach toward absorption, distribution, metabolism, and excretion of Xiaoke pills in zebrafish based on UPLC-HRMS and DESI-MS techniques

    Zhu, ChunyanJiang, XiaojuanTian, JuanjuanChen, Jiayun...
    9页
    查看更多>>摘要：Traditional Chinese medicine (TCM) has been used in clinical settings for over 2000 years in China. The study of the absorption, distribution, metabolism, and excretion (ADME) of TCM in vivo could be beneficial for the discovery of the active components in TCM. However, the conventional strategies used for ADME research are based on rodent models and have the characteristics of lengthy experimental periods, complex processes, and extensive data processing, which make it difficult to perform rapid analyses and high-throughput ADME screening of the medicinal components of TCM. In this study, an integrated high-throughput research strategy for the in vivo ADME analysis of TCM was established based on a zebrafish model. Accordingly, a combination of ultraperformance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS), desorption electrospray ionization-mass spectrometry (DESI-MS) imaging, and in-house non-targeted precise-and-thorough backgroundsubtraction (PATBS) data post-processing techniques were successfully applied for the analysis of the metabolism of zebrafish exposed to Xiaoke pills. A total of 49 compounds related to Xiaoke pills (including 13 prototypical components and 36 metabolites) were detected in zebrafish. In total, 32 of them, including puerarin, daidzein, deoxyschizandrin, formononetin, and glibenclamide, which have been identified to have hypoglycemic activity in our previous studies and are phase I and phase II metabolites resulting from the hydroxylation, demethylation, glucuronidation, sulfation, and glycosylation of the prototypical components in vivo, were found in rats treated with Xiaoke pills. Furthermore, the overall distribution of the known compounds in zebrafish exposed to Xiaoke pills was explored using DESI-MS. In summary, this study provides a practical approach for the high-throughput screening of the active components of TCM using a zebrafish model.
      原文链接:
    • NSTL
    • Elsevier

    Quantification of Glucose, fructose and 1,5-Anhydroglucitol in plasma of diabetic patients by ultra performance liquid chromatography tandem mass spectrometry

    Li, MengnaYan, DewenHao, MingyuHuang, Xiaohong...
    7页
    查看更多>>摘要：Type 2 diabetes mellitus (T2DM), a worldwide disease that affects the quality of human life and social development. Glucose, fructose and 1,5-anhydroglucitol are closely related to diabetes mellitus. However, few methods have been reported to achieve these three carbohydrates in the blood simultaneously. In this study, a UPLC-MS/MS method allowing to quantify glucose, fructose, and 1,5-anhydroglucitol simultaneously in human plasma was developed. The analysis was performed by UPLC-MS/MS system with HILIC column. This new method provided satisfactory results in terms of calibration curves with good linearity (R-2 > 0.99) over 3 order of magnitude range, precision (coefficient of variation of intra-day and inter-day: 0.72-10.23% and 2.21-13.8%), accuracy (results of intra-day and inter-day: 97-113%, 100-107%), matrix effects (87-109%), recovery (93-119%), carry-over (0.004-0.014%), as well as stability (0.04-6.9%) within the acceptance criteria. The reproducible, precise and accurate method with suitable dynamic ranges was successfully applied to the analysis of glucose, fructose and 1,5-anhydroglucitol in T2DM under different pathophysiological conditions.
      原文链接:
    • NSTL
    • Elsevier

    A rapid and sensitive method for the quantification of dopamine and serotonin metabolites in cerebrospinal fluid based on UHPLC with fluorescence detection

    Boulghobra, AyoubBonose, MyriamBillault, IsabellePallandre, Antoine...
    8页
    查看更多>>摘要：Inborn errors of dopamine and serotonin metabolism are diseases caused by deficiencies in enzymes belonging to metabolic pathways. The specific diagnosis of these inborn illnesses is based on the identification and quantification of biomarkers in cerebrospinal fluid (CSF), especially: 5-hydroxy-tryptophane (5-HTP), 5-hydroxy-indolacetic acid (5-HIAA), 3-ortho-methyl-DOPA (3-OMD), homovanillic acid (HVA) and 3-methoxy-4-hydroxyphenylglycol (MHPG). In the present work, we propose a novel ultrahigh performance liquid chromatography (UHPLC) method coupled to fluorescence detection (FD) to quantify simultaneously the five dopamine and serotonin metabolites. This method efficiently separates the five molecules in less than 10 min. A complete validation of the proposed method was performed in terms of accuracy, linearity, precision, and lower limit of quantification (LLOQ). Depending on the compound, the obtained LLOQs are between 1 nM and 5 nM, thus allowing to measure concentrations as low as in CSF samples. We also verified the method applicability by analyzing 10 CSF samples in triplicates. The obtained results showed satisfactory repeatability and an ability of this method to clearly distinguish healthy samples from pathologic samples, hence, demonstrating, the method suitability for diagnosing inborn errors of dopamine and serotonin metabolism. Therefore, the proposed UHPLC-FD method appears as a reliable alternative to the current gold standard for the quantification of these biomarkers, which is based on UHPLC coupled to electrochemical detection (ECD).
      原文链接:
    • NSTL
    • Elsevier

    Chemometrics-assisted development of a validated LC method for simultaneous estimation of temozolomide and gamma-linolenic acid: Greenness assessment and application to lipidic nanoparticles

    Beg, SarwarPanda, Sagar S.Singh, Kamalinder K.
    13页
    查看更多>>摘要：The described work entails the development of a simple, sensitive, green, and robust high-performance liquid chromatographic (HPLC) method for simultaneous estimation of temozolomide (TMZ) and gamma-linolenic acid (GLA). The chemometric factor screening study helped identify the critical method parameters optimized using Box-Behnken design for improved understanding and enhancing the method performance. Chromatographic separation was performed on a Kinetex (R) C-18 column (150 x 4.6 mm, 5 mu m particle size) using methanol: water (pH adjusted to 3.5 using 0.5% v/v O-phosphoric acid) as the mobile phase at 0.5 mL/min flow rate and diode array detection between 210 and 360 nm. The linearity of the method was observed for concentrations of TMZ and GLA ranging between 1 and 100 mu g.mL(-1) (R-2 = 0.999, p < 0.05). Accuracy evaluation showed good percent recovery within 97.9-100%, while intra- and inter-day precision showed RSD values within 0.37%-1.01%. The limit of detection and quantification for TMZ was found to be 0.75 and 1.0 mu g.mL(-1), respectively, while the values 0.55 and 1.0 mu g.mL(-1), respectively, were observed for GLA. System suitability (96.9-102.8%), its limits, and robustness evaluation indicated good percent recovery within, while RSD values were found to be within the acceptable limit of less than 2%. The method was specific for its ability to detect the analytes and their degradation products during forced degradation studies, which also indicated that TMZ was highly prone to alkaline conditions while GLA showed mild degradation in all the studied conditions. The estimation of both the analytes from lipid nanoparticles formulation showed good values for total drug content (82.6-85.3%), entrapment efficiency (95.4 to 98.7%), and drug loading (25.2 to 38.4%). Overall, the results indicated that the developed method was reliable for its accuracy, precision, sensitivity, and specificity for simultaneous estimation of the analytes. The method was found to be stability-indicating in nature and suitable for simultaneous estimation of TMZ and GLA from the developed nanoparticles formulation. Further, employing a greenness assessment approach established the method greenness.
      原文链接:
    • NSTL
    • Elsevier