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51.
Xiaoji Cao Jingfang Qiao Liping Wang Xuemin Ye Lebin Zheng Nan Jiang Weimin Mo 《Rapid communications in mass spectrometry : RCM》2012,26(7):740-748
A powerful ionic liquid‐based ultrasonic‐assisted extraction (ILUAE) method combined with ultra‐performance liquid chromatography coupled to electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry (UPLC/ESI‐QTOFMSn) was employed in the rapid simultaneous screening of iridoid glycosides, phenylethanoid glycosides, and cucurbitacin glycosides from P. scrophulariiflora. The ILUAE procedure was optimized over several ultrasonic parameters, including the ultrasonic power, concentration of the ionic liquid, and solid–liquid ratio. A comparison with conventional heat‐reflux extraction and regular UAE demonstrated that the optimized approach yielded a high extraction efficiency (Picroside I, 2.84%; Picroside II, 3.57%; 6‐O‐E‐feruloyl catalpol, 2.20%) within a short extraction time of 30 min. Negative ion mode ESI‐QTOFMS2 analysis of the fragmentation reactions of the [M–H]– ions was conducted to characterize the diagnostic ions related to the glycosyl moieties, aglycone units, and the type and substituted position of the ester groups. Interestingly, the positional isomers of the iridoid glycosides could be easily discriminated based on the characteristic ions. A total of 15 glycosides, including three groups of iridoid glycoside isomers and two groups of phenylethanoid glycoside isomers, were conveniently identified within 13.5 min. Moreover, 6'‐O‐vanilloyl catalpol was identified in P. scrophulariiflora for the first time. The method developed here was further validated by measuring the recovery, correlation coefficient (R2), and reproducibility (RSD, n = 5) of three iridoid glycosides: 89.60%–109.02%, 0.9991–0.9998, and 0.93%–1.44%, respectively. This study demonstrated the capabilities of ILUAE combined with UPLC/ESI‐QTOFMSn for the rapid screening of glycosides in P. scrophulariiflora. This method offers an approach to similar studies on other natural plants. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
52.
Shi‐jia Liu Ling Zhou Jun Zhang Chang‐yin Li Zi‐xiu Liu Wen‐zheng Ju 《Biomedical chromatography : BMC》2013,27(4):515-519
A highly sensitive liquid chromatography–tandem mass spectrometry method was developed and validated for the determination of limonin in beagle dog plasma using nimodipine as internal standard. The analyte and internal standard (IS) were extracted with ether followed by a rapid isocratic elution with 10 mm ammonium acetate buffer–methanol (26:74, v/v) on a C18 column (150 × 2.1 mm i.d.) and subsequent analysis by mass spectrometry in the multiple reaction monitoring mode. The precursor to product ion transitions of m/z 469.4 → 229.3 and m/z 417.2 → 122.0 were used to measure the analyte and the IS. The assay was linear over the concentration range of 0.625–100 ng/mL for limonin in dog plasma. The lower limit of quantification was 0.312 ng/mL and the extraction recovery was >90.4% for limonin. The inter‐ and intra‐day precision of the method at three concentrations was less than 9.9%. The method was successfully applied to pharmacokinetic study of limonin in dogs. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Quantitative study of cellular heterogeneity in doxorubicin uptake and its pharmacological effect on cancer cells
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Bin Deng Zhi‐Ming Wang Zi‐Hao Zhou Yi‐Meng Liu Xi‐Liang Yang Jian Song Yu‐Xiu Xiao 《Biomedical chromatography : BMC》2014,28(10):1393-1401
Cellular heterogeneity in doxorubicin (DOX) uptake and its relationship with pharmacological effect on cancer cells were quantitatively investigated for the first time. An in vitro experimental model was established by treating human leukemia K562 and breast cancer MCF‐7 cells with different schedules of DOX with or without surface P‐glycoprotein (P‐gp) inhibitor verapamil (VER). The cellular heterogeneity in DOX uptake was quantitatively examined by single‐cell analysis using capillary electrophoresis coupled with laser‐induced fluorescence detection. The corresponding cytotoxic effect was tested by cellular morphology, 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyl‐tetrazolium and flow cytometry assays. The expression of cellular membrane surface P‐gp was determined by flow cytometry. Results showed that the cellular heterogeneity exists in DOX uptake. The single‐high DOX schedule leads to lower uptake heterogeneity and higher mean drug uptake. The cellular heterogeneity in DOX uptake was found to be negatively correlated with drug cytotoxicity and surface P‐gp expression, with r = ?0.7680 to ~ ?0.9587. VER reduces the cellular variation in DOX uptake, suggesting that surface P‐gp may be one of the causes of the cellular heterogeneity in DOX uptake. This research demonstrates the importance of quantitative study of cellular heterogeneity in drug uptake and its potential application in drug schedule design, response prediction and therapy modulation. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
55.
A Comparative Study of Solutions of Silk Fibroin in 1-Butyl-3-methylimidazolium Chloride and Acetate
A. I. Susanin E. S. Sashina P. Ziółkowski V. V. Zakharov M. Zaborski M. Dziubiński P. Owczarz 《Russian Journal of Applied Chemistry》2018,91(4):647-652
A comparative study of the molecular-mass characteristics and rheological properties of solutions of silk fibroin in 1-butyl-3-methylimidazolium chloride and acetate was made. 相似文献
56.
Jun‐Yi Chen Zi‐Long Xiang Feng Yu Bert F. Sels Yu Fu Ting Sun Mario Smet Wim Dehaen 《Journal of polymer science. Part A, Polymer chemistry》2014,52(18):2596-2603
A series of hyperbranched polyacenaphthenequinones has been prepared by superelectrophilic aromatic substitution of (substituted) acenaphthenequinone and 1,3,5‐tris‐(4‐phenoxybenzoyl)benzene via a facile A2 + B3 approach. Because of the strongly increased reactivity of the second A functionality, gelation was efficiently avoided during the polymerization. The structure of the resulting polymer was characterized by NMR spectroscopy and gel permeation chromatography. Further modification of the hyperbranched polyacenaphthenequinone was explored both on the acenaphthenequinone and aromatic moieties. Moreover, the polymer modified through sulfonation was investigated as a water‐soluble acid catalyst for the degradation of biomass resources. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 2596‐2603 相似文献
57.
The ZnO catalysts supported on Silicalite‐1 zeolites with different crystallite sizes (0.08, 0.35, 1 and 1.7 μm, respectively) and 5% Zn were synthesized via an incipient wetness method. The catalysts were characterized by XRD, N2 adsorption, SEM, TEM‐EDX, DRIFT spectra and NH3‐TPD, and their catalytic performance in isobutane dehydrogenation assisted by CO2 was investigated. The catalytic activity is strongly dependent on the crystallite size of Silicalite‐1 support. The ZnO/S‐1‐0.35 catalyst with ca. 0.35 μm crystallite size displays the highest activity, affording an initial isobutane conversion of 51.0% and 74.5% isobutene selectivity. This can be attributed to a higher amount of acid sites present on this catalyst as well as the largest amount of nest silanols possessed by the S‐1‐0.35 support. 相似文献
58.
Wei Qinghua Li Zi Yang Xi Chen Jianghui Liu Xiaohua Hu Wenhao Liu Shunying 《Molecular diversity》2019,23(4):997-1010
Molecular Diversity - A Rh(I)/Sc(III) co-catalyzed synthesis of highly valuable functionalized 1,4-diketone derivatives in good yields and with an excellent diastereoselectivity. The established... 相似文献
59.
Cu‐doped Ni‐based metal–organic frameworks (MOFs) nanomaterials fabricated through a one‐pot hydrothermal reaction were characterized, and their performance as supercapacitor electrode materials was further studied for the first time. The results indicated that the doping of foreign metals and the introduction of K3[Fe(CN)6] in the KOH electrolyte significantly improve the performance of the supercapacitor. The results indicated that the Ni2.6Cu0.4 MOFs material shows the highest specific capacitance (1282 F g?1 at 1 A g?1 in mixed 2 M KOH and 0.1 M K3[Fe(CN)6]) and optimal capacitance retention (85.7% after 2000 cycles). This work provides a feasible optimization strategy for the construction of MOFs‐based supercapacitor electrode materials with excellent performance, and also provides a reliable experimental and theoretical basis for practical industrial production. 相似文献
60.