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Separation of cannabinoids on three different mixed‐mode columns containing carbon/nanodiamond/amine‐polymer superficially porous particles 下载免费PDF全文
Chuan‐Hsi Hung Janusz Zukowski David S. Jensen Andrew J. Miles Clayton Sulak Andrew E. Dadson Matthew R. Linford 《Journal of separation science》2015,38(17):2968-2974
Three mixed‐mode high‐performance liquid chromatography columns packed with superficially porous carbon/nanodiamond/amine‐polymer particles were used to separate mixtures of cannabinoids. Columns evaluated included: (i) reversed phase (C18), weak anion exchange, 4.6 × 33 mm, 3.6 μm, and 4.6 × 100 mm, 3.6 μm, (ii) reversed phase, strong anion exchange (quaternary amine), 4.6×33 mm, 3.6 μm, and (iii) hydrophilic interaction liquid chromatography, 4.6 × 150 mm, 3.6 μm. Different selectivities were achieved under various mobile phase and stationary phase conditions. Efficiencies and peak capacities were as high as 54 000 N/m and 56, respectively. The reversed phase mixed‐mode column (C18) retained tetrahydrocannabinolic acid strongly under acidic conditions and weakly under basic conditions. Tetrahydrocannabinolic acid was retained strongly on the reversed phase, strong anion exchange mixed‐mode column under basic polar organic mobile phase conditions. The hydrophilic interaction liquid chromatography column retained polar cannabinoids better than the (more) neutral ones under basic conditions. A longer reversed phase (C18) mixed‐mode column (4.6 × 100 mm) showed better resolution for analytes (and a contaminant) than a shorter column. Fast separations were achieved in less than 5 min and sometimes 2 min. A real world sample (bubble hash extract) was also analyzed by gradient elution. 相似文献
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Marcin Kubisiak Karolina Zelga Wojciech Bury Iwona Justyniak Krzysztof Budny-Godlewski Zbigniew Ochal Janusz Lewiński 《Chemical science》2015,6(5):3102-3108
This paper reports a series of comparative experiments on the activity of carbon- and oxygen-centred radical species in a model reaction of the radical addition of THF to imines mediated by a series of zinc alkyl/air reaction systems. The study strongly contradicts the notion that generally R˙ radicals are the initiating species in organic reactions mediated by RnM/air systems, and simultaneously demonstrates that oxygen-centred radical species are the key intermediates responsible for the initiation process. In addition, a new efficient RZn(L)/air initiating system for radical organic reactions exampled by a model reaction of radical addition of THF to imines is developed. Moreover, the isolation and structural characterization of the first zinc alkylperoxide supported by a carboxylate ligand, [Zn4(μ3-OOtBu)3(μ4-O)(O2CEt)3]2, as well as the novel octanuclear zinc oxo(alkoxide) aggregate with entrapped O–THF species, [Zn4(μ4-O)(μ3-2-O–THF)(O2CEt)5]2, provide clear mechanistic signatures for the mode of function of the RZn(O2CR′)/air system. 相似文献
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Magdalena Leśniak Marcin Gajek Janusz Partyka Maciej Sitarz 《Journal of Thermal Analysis and Calorimetry》2017,130(1):165-176
In this work, the structure and thermal properties of aluminosilicate fritted glazes in SiO2–Al2O3–CaO–MgO–Na2O–K2O–ZnO system with (4.0 mol%) and without addition of ZnO were examined by GIXRD, FTIR, MAS-NMR and thermal methods (DTA, DIL). It has been found that the all experimental glazes are amorphous material (transparent glazes). On the base of spectroscopic investigations, it was found that zinc ions exist in the network glazes in the octahedral coordination—Zn2+ ions play a network modifier role in structure of glazes. An analysis of the data obtained from thermal tests showed that addition of ZnO into chemical composition results in decrease in glass transition temperature value (T g) for all glazes (DTA, DIL). The coefficient of thermal expansion (α) is decreased as the whole measurement range for one series of fritted glazes. 相似文献
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Krzysztof Kaczmarek Barbara Pacholczyk-Sienicka ukasz Albrecht Janusz Zabrocki Ronald J. Nachman 《Molecules (Basel, Switzerland)》2021,26(11)
A facile solid-phase synthetic method for incorporating the imidazoline ring motif, a surrogate for a trans peptide bond, into bioactive peptides is reported. The example described is the synthesis of an imidazoline peptidomimetic analog of an insect pyrokinin neuropeptide via a cyclization reaction of an iminium salt generated from the preceding amino acid and 2,4-diaminopropanoic acid (Dap). 相似文献
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In vivo solid phase microextraction sampling of human saliva for non-invasive and on-site monitoring
Vincent Bessonneau Ezel BoyaciMalgorzata Maciazek-Jurczyk Janusz Pawliszyn 《Analytica chimica acta》2015
On-site sample preparation is an analytical approach based on direct sampling from the system under investigation. It has the advantage of combining sampling and sample preparation into a single step, thus generally is fast, minimizes the potential sources of error and eliminates the risks for analytes instability. For such analysis solid phase microextraction in thin film geometry (TF-SPME) can provide robust and convenient in vivo sampling, offering in the same time faster analysis and higher extraction recovery (i.e., better sensitivity) due to large surface to volume ratio. 相似文献
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Abdul Raheem Keeri Dr. Andrea Gualandi Prof. Dr. Andrea Mazzanti Prof. Dr. Janusz Lewinski Prof. Dr. Pier Giorgio Cozzi 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(52):18949-18952
The first catalytic asymmetric addition of TosMIC to unactivated ketones is presented. A combination of Me2Zn and aminoalcohol catalyst promoted the aldol addition/cyclization reaction to render oxazolines possessing a fully substituted stereocenter with excellent yields (up to 92 %), high enantioselectivities (up to 96 %), and complete diastereoselectivity. The chiral oxazolines were then used to give, after a straightforward acid hydrolysis, enantioenriched building blocks bearing tertiary alcohol motifs such as hydroxylaldehydes, hydroxylacids, and hydroxylesters without racemization. 相似文献
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Theoretical model for deformability of brittle rock-like materials in the presence of an oriented damage of their internal structure is formulated and verified experimentally. This model is based on the assumption that non-linearity of the stress–strain curves of these materials is a result of irreversible process of oriented damage growth. It was also assumed that a material response, represented by the strain tensor, is a function of two tensorial variables: the stress tensor and the damage effect tensor that is responsible for the current state of the internal structure of the material. The explicit form of the respective non-linear stress–strain relations that account for the appropriate damage evolution equation was obtained by employing the theory of tensor function representations and by using the results of own experiments on damage growth. Such an oriented damage that grows in the material, described by the second order symmetric damage effect tensor, results in gradual development of the material anisotropy. The validity of the constitutive equations proposed was verified by using the available experimental results for concrete subjected to the plane state of stress. The relevant experimental data for sandstone and concrete subjected to tri-axial state of stress were also used. 相似文献