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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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    A fabric phase sorptive extraction method for the LC-UV determination of bisphenol A and leaching monomers from dental materials in human saliva

    Andreasidou, EiriniMourouzis, PetrosDaktylidi, LoukiaKabir, Abuzar...
    9页
    查看更多>>摘要：A rapid and simple fabric phase sorptive extraction (FPSE) procedure is developed for the simultaneous extraction of four monomers (Bisphenol A, BPA; Triethylene glycol dimethacrylate, TEGDMA; Urethane dimethacrylate, UDMA; Bisphenol A-glycidyl methacrylate, BisGMA) in human saliva, prior to the determination by high pressure liquid chromatography with an ultraviolet-visible detector. FPSE is a green sample preparation technique, harmonized with the principles of Green Analytical Chemistry (GAC), which utilizes a flexible surface, such as cellulose, chemically coated with a polymeric material using sol-gel technology. FPSE membranes are characterized by superior chemical stability and any solvent or solvent mixture can be used for elution. Among twelve different sol-gel coated membranes, an FPSE membrane coated with sol-gel polytetrahydrofuran (sol-gel PTHF) was found optimum to extract four target compounds from saliva samples, which were first centrifuged. Parameters with most significant impact on the extraction efficiency of FPSE including elution solvent, utilization of magnetic stirring, extraction time have been comprehensively studied and optimized. The studied compounds' separation was carried out by a Perfect Sil 120 ODS-2 chromatographic column (250 mm x 4.0 mm, 5 mu m), using a mobile phase constituting of acetonitrile-water 70:30 % v/v (isocratic elution). The total analysis time was 10 min. Detection was achieved by an ultraviolet-visible detector at 220 nm. The method was validated in terms of sensitivity, linearity, trueness, precision, selectivity and stability of samples. For all four compounds, the limit of detection and the limit of quantification were 0.075 ng/mu L and 0.25 ng/mu L, respectively. Relative recovery rates were between 90.0 and 106.7%, while RSD values were < 8.1 and 12% for interday and intraday repeatability, respectively. Youden & Steiner approach was applied to study method's ruggedness and reusability of the media was tested, which enhanced the green nature of technique.
      原文链接:
    • NSTL
    • Elsevier

    Simultaneous determination of febuxostat and montelukast in human plasma using fabric phase sorptive extraction and high performance liquid chromatography-fluorimetric detection

    Gazioglu, IsilTekkeli, S. Evrim KepekciTartaglia, AngelaAslan, Ceylin...
    8页
    查看更多>>摘要：In the present work, a new sensitive and selective high-performance liquid chromatography-fluorimetric detection (HPLC-FLD) method was developed and validated to quantify febuxostat (FBX) and montelukast (MON) in human plasma. The developed procedure was successfully applied to a study aimed at evaluating the pharmacokinetic profiles of febuxostat and montelukast in human plasma. A sol-gel poly (caprolactone)-block- poly(dimethylsiloxane)-block-poly(caprolactone) (sol-gel PCAP-PDMS-PCAP) extraction sorbent coated fabric phase sorptive extraction membrane was used in the extraction process. The entire chromatographic analysis was performed with isocratic elution of the composition of the mobile phase (acetonitrile:water, 60:40, v:v, 0.032% glacial acetic acid) on the C18 column. The flow rate is varied during the analysis, particularly from 0.5 mL min(-1) at the start and linearly increased to 1.5 mL min(-1)& nbsp;in 7 min. The detection and quantification of the analytes was carried out by means of a fluorimetric detector at 320 nm and 350 nm as absorption wavelengths and at 380 and 400 nm as emission wavelengths for FBX and MON, respectively. The calibration curves demonstrated linearity in the range 0.3-10 ng mL(-1)& nbsp;and 5-100 ng mL(-1)& nbsp;for FBX and MON, respectively, while the LOD and LOQ values were 0.1 and 0.3 ng mL(-1)& nbsp;for FBX and 1.5 and 5 ng mL(-1)& nbsp;for MON. Intraday and interday RSD% values were found lower than 5.79%. As reported, the method was applied to real plasma samples obtained from a volunteer who was co-administered both the drugs. Pharmacokinetic data reveal that the concentration of both the drugs reaches the plateau approximately at the same time, but exhibits an elimination phase at different rates. This study demonstrated the usefulness of the new method and its applicability in therapeutic drug monitoring (TDM).
      原文链接:
    • NSTL
    • Elsevier

    New method for screening anti-Leishmania compounds in plants extracts by HPTLC-bioautography

    Hilaire, ValentinMichel, GregoryMajoor, AlissaHadji-Minaglou, Francis...
    5页
    查看更多>>摘要：Leishmania genus is responsible for leishmaniasis, a group of diseases affecting 12 million people in the tropical and subtropical zone. Currently, the few drugs that are available to treat this disease are expensive and cause many side effects. Searching for new therapeutics from plant species seems to be a promising path. This work proposes an original HPTLC test against parasites, in particular on Leishmania infantum, to screen new molecules from plant extracts. The technique uses protozoa transformed to express the luciferase gene to observe the bioautogram in bioluminescence. We have developed two different test protocols based on the two dimorphic stages of the parasite. The free promastigote stage, and an intracellular stage parasitizing macrophage cells called the amastigote stage. These two stages only survive under extremely different conditions which required the development of two very different test protocols. For the promastigote free stage of the protozoa, the direct bioautography technique was chosen while for the intracellular amastigote stage, bioautography by immersion (agar overlay) was required. Amphotericine B was chosen as the reference compound for this assay. The development of each of these two tests made it possible to clearly detect areas of activity on the bioautogram, allowing a rapid and inexpensive screening of the antiparasitic properties of molecules in natural extracts.
      原文链接:
    • NSTL
    • Elsevier

    Selective extraction of gambierone and related metabolites in Gambierdiscus silvae using m-aminophenylboronic acid-agarose gel and liquid chromatography-high-resolution mass spectrometric detection

    Mudge, Elizabeth M.Robertson, AlisonLeynse, Alexander K.McCarron, Pearse...
    12页
    查看更多>>摘要：Gambierdiscus spp. are epi-benthic dinoflagellates that have been associated with ciguatera poisoning. These microalgae can have complex secondary metabolite profiles including ciguatoxins, maitotoxins, and gambierones, with varying compositions and toxicities across species and strains. Given this chemical diversity there is a need to develop selective and sensitive methods for secondary metabolite profiling. In this study, we used a cultured Caribbean strain of Gambierdiscus silvae to develop sample preparation and analysis strategies for characterizing vic-diol containing secondary metabolites. A pooled cellular extract was first screened by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) for ciguatoxin-related compounds, which resulted in the confirmation of gambierone (1) and a novel isomer of 44-methylgambierone (3). Treatment of the extract with periodate confirmed that the gambierones each contained one reactive vic-diol, which was exploited for the development of a selective extraction procedure using m-aminophenylboronic acid gel and the non aqueous binding solvent chloroform. Using this non-traditional boronate affinity procedure, LC-HRMS also revealed the presence of additional sulfated polycyclic ethers in the gambierone-containing vic-diol fraction, while pigments and other contaminants were removed. The developed tools could be applied to screen collections of Gambierdiscus and other benthic algae to provide additional chemical characterization of gambieronerelated compounds. The selective extraction procedure may also prove useful as a step in the isolation of these sulfated polyethers for structural, toxicological and biotransformation studies.
      原文链接:
    • NSTL
    • Elsevier

    An integrated chemical characterization based on FT-NIR, GC-MS and LC-MS for the comparative metabolite profiling of wild and cultivated agarwood

    Yao, ChengQi, LumingZhong, FurongLi, Na...
    10页
    查看更多>>摘要：Agarwood is a well-known and precious traditional Chinese medicine, has been widely applied as drugs and spices for century. The large demand for this material has deeply stimulated the emergence of numerous cultivated products. However, it is difficult to distinguish wild agarwood from cultivated agarwood, and the chemical composition difference between them is not clear. In this study, an integrated method of Fourier transform near-infrared (FT-NIR), gas chromatography-mass spectrometry (GC-MS) and ultraperformance liquid chromatography Quadrupole-Exactive Orbitrap tandem mass spectrometry (UHPLC-Q-Exactive Orbitrap/MS) was developed to explore chemical variation between wild and cultivated agarwood in combination with multivariate statistical analysis. Twenty-four wild and cultivated agarwood samples were collected from different regions. FT-NIR profiles were used to obtain the holistic metabolic characterization in combination with principal component analysis (PCA). A total of seventy-six and seventy-nine metabolites, including volatile components and 2-(2-phenethyl) chromones derivatives, were successfully identified by GC-MS and UHPLC-QExactive Orbitrap/MS, respectively. Thereafter, the orthogonal-partial least square method-discriminant analysis (OPLS-DA) and variable importance in the projection (VIP) were used to screen potential characteristic chemical components (VIP > 1) in wild and cultivated agarwood, respectively. Finally, eight key chemical markers were putatively identified by two techniques to distinguish agarwood from different origins, which can be found that sesquiterpenes, aromatics, terpenoids, 2-(2-phenylethyl) chromones of the flidersia type (FTPECs) and tetrahydro-2-(2-phenylethyl) chromones (THPECs) are the most important metabolites. Summary, this research presented a comprehensive metabolomic variation between wild and cultivated agarwood on the basis of a multi-technology platform, which laid a foundation for distinguishing the two ecotypes of agarwood and was conducive to the quality control of this resource.
      原文链接:
    • NSTL
    • Elsevier

    Study of antifungal agent caspofungin adsorption to laboratory materials

    Ramirez-Garcia, A.Rementeria, A.Ba, B. B.Gaudin, K....
    8页
    查看更多>>摘要：Treatment of invasive fungal infections with Caspofungin is used as the first-line antifungal agents. The minimum inhibitory concentration value is a test which indicates the degree of sensitivity of a strain regarding a drug. However, no value of minimum inhibitory concentration for caspofungin is available because very variable value is obtained. In this work, we study the link with the adsorption phenomenon of CSF previously described in literature and the lack of minimum inhibitory concentration value.A systematic study of the impact of different parameters on CSF adsorption is reported. The effect of the nature of container material, the aqueous solution pH and the organic solvent proportion was studied. In addition, the possibility of using a coating agent to minimize the adsorption was assayed and evaluated.Results obtained showed the importance of the material used during the manipulation of CSF. The use of acidic pH aqueous solution or the addition of acetonitrile or methanol proportions (50 % and 70 %, respectively) were found efficient to avoid adsorption of CSF on glassware material, which is the relevant strategy for analytical samples of caspofungin. The treatment of HPLC glass vials and 96-well plates with N-(2-aminoethyl)-3-aminopropyltrimethoxysilane reduced the adsorption. The significant adsorption observed in this work especially with plastic materials, questions the results obtained before in different assays and explained the absence of MIC value.
      原文链接:
    • NSTL
    • Elsevier

    Screening of blood-activating active components from Curcuma wenyujin Y. H. Chen et C. Ling rhizome based on spectrum-effect relationship analysis and network pharmacology

    Zhao, MengtingHao, MinTong, HuangjinSu, Lianlin...
    12页
    查看更多>>摘要：Curcuma wenyujin Y.H. Chen et C. Ling rhizome (also called EZhu in China) has long been used as plant medicine for its traditional effect on promoting blood circulation and remove blood stasis. However, the active components of EZhu are still unclear at present. This research is managed to investigate the pharmacodynamics material basis on removing blood stasis of EZhu by exploring the spectrum-effect relationship between UPLC-Q/TOF-MS fingerprints and pharmacologic actions. Hemorheology and related functional parameters were detected to evaluate the pharmacologic actions of EZhu. Relative content Changes of components in rat plasma were detected by UPLC-Q/TOF-MS. A compound-target-pathway network was built to predict the pharmacological activity of components in plasma. Then, bivariate correlation analysis (BCA) was used to explore the correlation degree between components in plasma and pharmacologic actions of EZhu. In UPLC-Q/TOF-MS fingerprints of rat plasma, 10 prototype components were identified. BCA results show that 8 components were concerned with the pharmacological activity for treating blood stasis syndrome (BSS) in varying degrees (R > 0.5, P < 0.05). Among them, zedoarofuran and curzerenone have shown correlation with more pharmacological indicators. The network predicted that 80 targets were closely related to 10 components, in which 48 targets were connected with 159 metabolic pathways including arachidonic acid metabolism, sphingolipid signaling pathway, and linoleic acid metabolism. Overall, this study provided a scientific basis for TCM quality control to ensure its safety and efficacy.
      原文链接:
    • NSTL
    • Elsevier

    A validated method for the separation of ethyl glucoside isomers by gas chromatography-tandem mass spectrometry and quantitation in human whole blood and urine & nbsp;

    Waters, BrianNakano, RyokoHara, KenjiMatsusue, Aya...
    7页
    查看更多>>摘要：Ethyl glucoside (EG) is present in Japanese sake in high concentrations, and can be found in other alcoholic beverages like beer and wine in varying amounts. EG exists as alpha (alpha) and beta (beta) isomers, and the concentrations and ratios of these isomers differ depending on the alcoholic beverage. Herein, we report a validated analysis method for the separation of EG isomers in human whole blood and urine, by GC-MS/MS. Whole blood and urine samples were deproteinized and interferences removed by weak cation exchange cartridges. The target analytes were acetylated using acetic anhydride and pyridine by microwave-accelerated derivatization. Sepa-ration was performed using tandem columns, with detection in the multiple reaction monitoring (MRM) mode. The MRM transitions for all compounds were m/z 157.0 > 115.1 for the quantifying transition, and m/z 157.0 > 73.1 and m/z 141.0 > 81.0 for the qualifying transitions. Assay validation included linearity, LOD and LLOQ, bias, within-run and between-run precision, stability, and dilution integrity. Baseline separation of the 2 isomers was achieved with linear calibration (r(2) > 0.99) across the calibration range 0.625 to 50 mu g/mL for both alpha-and beta-EG in both whole blood and urine. The validated method was then applied to actual human whole blood and urine samples collected at autopsy, as well as relevant alcoholic beverage samples. The quantitation of EG isomers could benefit the forensic toxicology community by acting as markers for recent alcoholic beverage consumption.& nbsp;
      原文链接:
    • NSTL
    • Elsevier

    Isolation of achiral aliphatic acid derivatives from Piper kadsura using preparative two-dimensional chiral supercritical fluid chromatography

    Dai, ZhuoshunJiang, DasenDai, YingpingGe, Dandan...
    6页
    查看更多>>摘要：The separation of structural analogues in natural products has always been one of the challenges in separation science, where supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an unconven-tional but potential solution. In this study, a preparative two-dimensional chiral SFC (2D cSFC) method that was established with two kinds of CSPs was applied in the isolation of the aliphatic acid derivatives in Piper kadsura (P. kadsura). The RPLC unseparated peaks of two samples A and B of P. kadsura were evenly scattered on the CSP-1 column while they clustered into two groups on the CSP-2 column by SFC. There was impressively comple-mentary selectivity between CSP-1 and CSP-2, which were used for construction of 2D cSFC. The first dimension (D-1) separation with CSP-1 fractionated the sample A into six parts by a heart-cutting method and the sample B into nine parts for a comprehensive 2D analysis; then 29 and 71 peaks were respectively found in these parts in the second dimension (D-2) separation with CSP-2. Further through 2D preparative separation, 19 high purity components were obtained, and the chemical structures of two of them were confirmed, including a novel un-saturated aliphatic acid compound (8Z,10Z)-12-methoxyheptadeca-8,10-dienoic acid and a known octadeca-dienoic acid lactone Lactariolide. The 2D cSFC method presented the superiority of separating the achiral compounds of complex samples.
      原文链接:
    • NSTL
    • Elsevier

    Black raspberry extract shifted gut microbe diversity and their metabolic landscape in a human colonic model

    Zhang, ShiqiXu, MengyangSun, XiaoweiLiu, Xuyu...
    9页
    查看更多>>摘要：Human gut microbiota is critical for human health, as their dysbiosis could lead to various diseases such as irritable bowel syndrome and obesity. Black raspberry (BRB) has been increasingly studied recently for its impact on gut microbiota as a rich source of phytochemicals (e.g., anthocyanin). To investigate the effect of BRB extract on the gut microbiota composition and their metabolism, an in-vitro human colonic model (HCM) was utilized to study the direct interaction between BRB and gut microbiome. Conditions (e.g., pH, temperature, anaerobic environment) in HCM were closely monitored and maintained to simulate the human intestinal system. Fresh fecal samples donated by three young healthy volunteers were used for gut microbiota inoculation in the HCM. 16S ribosomal DNA sequencing and liquid-chromatography mass spectrometry (LC/MS) based metabolomics were performed to study the impact of BRB on gut microbiota characteristics and their metabolism (fatty acids, polar metabolites, and phenolic compounds). Our data suggested that BRB intervention modulated gut micro biota at the genus level in different HCM sections mimicing ascending, transverse, and descending colons. Relative abundance of Enterococcus was commonly decreased in all colon sections, while modulations of other bacteria genera were mostly location-dependent. Meanwhile, significant changes in the metabolic profile of gut microbiota related to fatty acids, endogenous polar metabolites, and phenolic compounds were detected, in which arginine and proline metabolism, lysine degradation, and aminoacyl-tRNA biosynthesis were mostly regulated. Moreover, we identified several significant associations between altered microbial populations and changes in microbial metabolites. In summary, our study revealed the impact of BRB intervention on gut microbiota composition and metabolism change, which may exert physiological change to host metabolism and host health.
      原文链接:
    • NSTL
    • Elsevier