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1.
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   

2.
The established analytical method for determining the concentration of dantrolene sodium (Da) in rat tissues by HPLC/MS/MS technique was successfully applied to tissue distribution studies of Da in rats. Tissue homogenate samples were pretreated by protein precipitation with pre‐cooled methanol. Chromatographic separation was achieved on an Acquity HPLC column (Kromat Universil XB‐C18, 2.1 × 150 mm, 3 μm). Mass spectrometry was conducted with an electrospray ionization interface in negative ionization mode and multiple reaction monitoring was used for quantitative analysis. The results showed that Da was rapidly and widely distributed in tissues and reached the maximum concentration within 0.5 h in all tissues after oral administration of Da–hydroxypropyl‐β‐cyclodextrin (DHC). It was then metabolized by liver and finally excreted from kidney,which indicated that DHC inclusion complex has better absorption and higher oral bioavailability than Da. The results also provided evidence for the safety and effectiveness of drug clinical application.  相似文献   

3.
Several silica‐based solutions with 50 g/l of SiO2 were prepared from sodium silicate solutions and silica sol; the silicate conversion coatings were obtained by immersing hot‐dip galvanized steel sheets in these solutions. These solutions were characterized using high‐resolution transmission electron microscopy and 29Si nuclear magnetic resonance; the morphology of the coatings was observed by SEM and atomic force microscopy while the corrosion resistance was evaluated by electrochemical measurements as well as neutral salt spray tests. The results show that the coatings obtained from the single silica sol solution had poor adhesion and the coating obtained from the sodium silicate solution with low SiO2/Na2O molar ratio was uneven. By adding the silica sol to the silicate solution with low molar ratio, uniform coatings with better protection property were obtained. According to the results of 29Si nuclear magnetic resonance spectra, the effects of the distribution of silicate anions with various polymerization degrees in the silica‐based solutions on the microstructure and corrosion resistance of the silicate coatings are discussed. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

4.
Elution profiles of kynurenic acid (KYNA) and 7‐chlorokynurenic acid (Cl‐KYNA) were examined by high‐performance liquid chromatography (HPLC) using a triazole‐bonded stationary phase column (Cosmosil® HILIC) under isocratic elution of a mobile phase consisting of CH3CN–aqueous 10 mm ammonium formate between pH 3.0 and 6.0. The capacity factors of KYNA and Cl‐KYNA varied with both the CH3CN content and the pH of the mobile phase. The elution order of KYNA and Cl‐KYNA was reversed between the CH3CN‐ and H2O‐rich mobile phases, suggesting that hydrophilic interactions and anion‐exchange interactions caused retention of KYNA and Cl‐KYNA in the CH3CN‐ and H2O‐rich mobile phases, respectively. The present HPLC method using a triazole‐bonded column and fluorescence detection (excitation 250 nm, emission 398 nm) was applied to monitor in vitro production of KYNA from d ‐kynurenine (d ‐KYN) by d ‐amino acid oxidase (DAO) using Cl‐KYNA as an internal standard. A single KYNA peak was clearly observed after enzymatic reaction of d ‐KYN with DAO. Production of KYNA from d ‐KYN was suppressed by the addition of commercial DAO inhibitors. The present HPLC method can be used to evaluate DAO activity and DAO inhibitory effects in candidate drugs for the treatment of schizophrenia. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

5.
A specific and sensitive HPLC‐MS/MS method was developed and validated for the simultaneously quantification of isoliquiritigenin (ISL) and neoisoliquiritin (NIS) in rat plasma by oral administration. Analytes were analyzed on an Agilent 6460 LC‐MS/MS system (Agilent, USA) using an Agilent Zorbax SB‐C18 column (4.6 × 150 mm, 5 μm). Gradient elution was applied for the analyte separation using a mobile phase composed of 0.1% formic acid aqueous solution and methanol at a flow rate of 1.0 mL/min with a total running time of 12 min. The calibration curves for ISL and NIS showed good linearity in the concentrations ranging from 0.001 to 4.000 μg/mL with correlation coefficients >0.998. The precision, accuracy, recovery and stability were deemed acceptable. The method was applied to the pharmacokinetics study of ISL and NIS in rats by single and combination administration. The result showed that Cmax and AUC0→t of ISL were markedly increased from 0.53 to 1.20 μg/mL, and from 69.63 to 200.74 min μg/mL by combination administration. The mean t1/2 value was also prolonged from 64.55 to 203.74 min in the combination group. These results indicated that NIS may have been metabolized to ISL which increased the absorption and extended the elimination of ISL. However, little difference was found for NIS pharmacokinetics parameters between single NIS and the combination group, which suggested that there was no significant biotransformation of ISL to NIS. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

6.
Liquid chromatographic assays were developed using a mixed‐mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve‐mediated column switching and was based upon a single high‐performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion‐exchange, (ii) mixed‐mode interactions under an applied dual gradient (reversed‐phase/ion‐exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed‐mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well‐resolved unknown peaks.  相似文献   

7.
Two unprecedented mixed BIII/PV complexes of meso‐triaryl 25‐oxasmaragdyrins were synthesized in appreciable yields under mild reaction conditions. These unusual 25‐oxasmaragdyrin complexes containing one or two seven‐membered heterocyclic rings comprised of five different atoms (B, C, N, O, and P) were prepared by reacting B(OH)(Ph)‐smaragdyrin and B(OH)2‐smaragdyrin complexes, respectively, with POCl3 in toluene at reflux temperature. The products were characterized by HRMS and 1D‐ and 2D‐NMR spectroscopy. X‐ray crystallography of one of the mixed BIII/PV smaragdyrin complexes indicated that the macrocycle is significantly distorted and contains a stable seven‐membered heterocyclic ring within the macrocycle. The bands in the absorption and emission spectra were bathochromically shifted with reduced quantum yields and singlet‐state lifetimes relative to the free base, meso‐triaryl 25‐oxasmaragdyrin. The mixed BIII/PV complexes were difficult to oxidize but easier to reduce than the free base. The DFT‐optimized structure of the 25‐oxasmaragdyrin complex with two seven‐membered heterocycles indicated that it was a bicyclic spiro compound with two half‐chair‐like conformers. This was in contrast to the chair‐like conformation of the complex with a single seven‐membered heterocyclic ring. Moreover, incorporation of a second phosphate group in the former case stabilized the bonding geometry and resulted in higher stability, which was reflected in the bathochromic shift of the absorption spectra, more‐positive oxidation potential, and less‐negative reduction potential.  相似文献   

8.
A new method for deposition nitrogen‐doped TiO2 nanofibers films was proposed. By using atmospheric pressure plasma jet generated by dual‐frequency power sources, the morphologies of these TiO2 films were investigated by scanning electron microscopy. The structures of these films were characterized by X‐ray diffraction and Raman Shift Spectroscopy. The elemental composition of these films [Colour figure can be viewed at wileyonlinelibrary.com ] were characterized by means of X‐ray photoelectron spectroscopy. The optical absorption of these films were studied by UV‐vis absorbance spectra. These results indicated that the nitrogen‐doped nanofibers TiO2 films have mixed phases of anatase and rutile. They also display narrow band gap. The I‐V characteristics curves exhibited good conductivity ability. Optical emission spectroscopy (OES) was measured to analyze the active group.  相似文献   

9.
We present an experimental investigation of the conformation and microstructure of Poly(N‐isopropylacrylamide) (PNIPA) in aqueous solution in the presence of salts. As a model, a strong salting–out salt (Na2SO4) and a strong salting–in salt (NaSCN) were chosen. Light scattering measurements show that Na2SO4 decreases the radius of gyration of PNIPA compared to its value in water, whereas NaSCN increases it. Moreover, the NaSCN solution was found to be a better solvent for PNIPA compared to water, whereas Na2SO4 solution is worse. Small‐angle neutron scattering measurements of semidilute PNIPA solutions, at temperatures well below the phase‐transition temperature, exhibit the behavior predicted by the model of dynamic concentration fluctuations characterized by a single correlation length. Excess scattering at low angles is observed in salt solutions at temperatures that are near, yet below, the phase‐transition temperature. This may indicate intrachain heterogeneities on the scale of 6–8 nm. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 3713–3720, 2004  相似文献   

10.
《Fluid Phase Equilibria》2005,231(2):150-162
The equilibrium of CO2 and carbamate concentration data for the absorption of CO2 in aqueous solutions of single and mixed amines was analyzed using the Deshmukh–Mather model. Data on CO2 loading in aqueous solutions of DEA and MDEA and their mixtures at various temperature (303–323 K) and CO2 partial pressure (0.09–100 kPa) together with carbamate concentrations in case of DEA and its mixtures with MDEA were fitted simultaneously to generate the different interaction parameters required to calculate the activity coefficients in the model. Using the generated interaction parameters, the model was applied to correlate the CO2 loading in solutions of DEA and MDEA and their mixtures reported in the literature as well as those obtained in our laboratory and was found to be able to give a good estimation of CO2 loading and carbamate concentration over a wide range of operating conditions in both single and mixed amine solutions.  相似文献   

11.
The aim of this study was to investigate the effects of verapamil on the pharmacokinetics of pristimerin in rats. A sensitive and reliable LC‐MS/MS method was developed and applied for the determination of pristimerin in rat plasma. The pharmacokinetics of orally administered pristimerin with and without verapamil pretreatment was investigated. The results indicated that, when the rats were pretreated with verapamil, the peak concentration of pristimerin increased from 189.13 to 277.53 ng/mL (46.7%), and the AUC0–t increased by approximately 82.0%. Additionally, the effects of verapamil on the absorption and metabolic stability of pristimerin were investigated using the Caco‐2 cell transwell model and rat liver microsomes. A markedly higher transport of pristimerin across the Caco‐2 cells was observed in the basolateral‐to‐apical direction and was abrogated in the presence of the P‐gp inhibitor, verapamil. These results indicated that P‐gp might be involved in the absorption of pristimerin. Of note, the metabolic half‐life of pristimerin was prolonged by the pretreatment with verapamil. In conclusion, verapamil could affect the pharmacokinetics of pristimerin, and it might work through increasing the absorption of pristimerin by inhibiting P‐gp, or through slowing down the metabolism of pristimerin in the rat liver. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

12.
Highly soluble hexadecaaniline (A16)‐grafted polyolefin derivatives poly(maleic acid‐hexadecaanilinamide‐alt‐1‐octadecene) (PMAO‐A16) in a comb‐like configuration with alternate linear hexadecane and A16 side‐chains were synthesized and characterized. The structure of PMAO‐A16 was substantiated by infrared and UV‐Vis spectra showing high intensity of characteristic absorption peaks corresponding to a high degree of A16 attachments. Covalent grafting of hexadecaanilines onto the polymer backbone of PMAO was confirmed by the detection of a new amide [–(C[dbnd]O)–NH–] absorption band appearing at 1661 cm?1 accompanied with the full disappearance of anhydride carbonyl absorptions. Based on the comparison between TGA profiles of PMAO‐A16 and hexadecaaniline, a 12.5% wt loss at 365–600°C was accounted for full elimination of aliphatic side‐chains that matches approximately with the weight percentage of total hexadecane arms (12.7%). The data revealed a nearly quantitative yield of A16 grafting on anhydride subunits leading to complete conversion of PMAO into PMAO‐A16. Furthermore, preliminary 1H‐NMR study of PMAO‐A16 indicated its capability to undergo molecular self‐assembly in DMSO where A16s were dispersed in the solvent phase with hexadecane side‐chains located in a phase‐separated domain.  相似文献   

13.
In vivo absorption and oxidative metabolism of salicylic acid in rat small intestine was studied by luminal perfusion experiment. Perfusion through the lumen of proximal jejunum with isotonic medium containing 250 μm sodium salicylate was carried out. Absorption of salicylate was measured by a validated HPLC‐DAD method which was evaluated for a number of validation characteristics (specificity, repeatability and intermediate precision, limit of detection, limit of quantification, linearity and accuracy). The method was linear over the concentration range 0.5–50 μg/mL. After liquid–liquid extraction of the perfusion samples oxidative biotransformation of salicylate was also investigated by HPLC‐MS. The method was linear over the concentration range 0.25–5.0 μg/mL. Two hydroxylated metabolites of salicylic acid (2,5‐dihydroxybenzoic acid and 2,3‐dihydroxybenzoic acid) were detected and identified. The mean recovery of extraction was 72.4% for 2,3‐DHB, 72.5% for 2,5‐DHB and 50.1% for salicylic acid, respectively. The methods were successfully applied to investigate jejunal absorption and oxidative metabolism of sodium salicylate in experimental animals. The methods provide analytical background for further metabolic studies of salycilates under modified physiological conditions.  相似文献   

14.
Hierarchical macro‐/mesoporous N‐doped TiO2/graphene oxide (N‐TiO2/GO) composites were prepared without using templates by the simple dropwise addition mixed solution of tetrabutyl titanate and ethanol containg graphene oxide (GO) to the ammonia solution, and then calcined at 350 °C. The as‐prepared samples were characterized by scanning electron microscopy (SEM), Brunauer‐Emmett‐Teller (BET) surface area, X‐ray diffraction (XRD), Raman spectroscopy, X‐ray photoelectron spectroscopy (XPS), and UV‐Vis absorption spectroscopy. The photocatalytic activity was evaluated by the photocatalytic degradation of methyl orange in an aqueous solution under visible‐light irradiation. The results show that N‐TiO2/GO composites exhibited enhanced photocatalytic activity. GO content exhibited an obvious influence on photocatalytic performance, and the optimal GO addition content was 1 wt%. The enhanced photocatalytic activity could be attributed to the synergetic effects of three factors including the improved visible light absorption, the hierarchical macro‐mesoporous structure, and the efficient charge separation by GO.  相似文献   

15.
A functionalized cyclic carbonate monomer containing a cinnamate moiety, 5‐methyl‐5‐cinnamoyloxymethyl‐1,3‐dioxan‐2‐one (MC), was prepared for the first time with 1,1,1‐tri(hydroxymethyl) ethane as a starting material. Subsequent polymerization of the new cyclic carbonate and its copolymerization with L ‐lactide (LA) were successfully performed with diethyl zinc (ZnEt2) as initiator/catalyst. NMR was used for microstructure identification of the obtained monomer and copolymers. Differential scanning calorimetry (DSC) was used to characterize the functionalized poly(ester‐carbonate). The results indicated that the copolymers displayed a single glass transition temperature (Tg) and the Tg decreased with increasing carbonate content and followed the Fox equation, indicative of a random microstructure of the copolymer. The photo‐crosslinking of the cinnamate‐carrying copolymer was also demonstrated. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 161–169, 2009  相似文献   

16.

The rheological properties of surfactant solutions are the main parameter that affects the surfactant application. In this work, the rheology of the mixed system 12‐3‐12,2Br?/SDS/H2O was discussed particularly. The relationship between the microstructure of surfactant aggregates and rheology of mixed solutions was explored. It is shown that the rheological properties of solutions have different behaviors at different molar ratio of two surfactants under given total concentration. With the increase of molar ratio (12‐3‐12,2Br?/SDS), the solution change from Newtonian liquid into positive thixotropy then to negative thixotropy, at last turn to positive thixotropy again, and ATPS becomes the dividing line. The difference of rheological properties is the embodiment of difference for surfactant aggregates' microstructures. The cryo‐TEM results shown that the solutions containing aggregates with big size, such as rodlike micelles, multilamellar micelles, show positive thixotropy. However, the solutions containing lamellar micelles or liquid crystal will show negative thixotropy. The positive thixotropy endows the mixied system a potential application in enhanced oil recovery.  相似文献   

17.
A novel, sensitive and reliable ultra fast liquid chromatography‐tandem mass spectrometry (UFLC‐MS/MS) method has been developed and validated for simultaneous quantitation of eight main active ingredients (evodiamine, rutaecarpine, dehydroevodiamine, limonin, ginsenoside Rb1, Rd, Re and Rg1) in rat plasma after oral administration of Wu‐Zhu‐Yu (WZY) decoction, which is a celebrated and widely used Traditional Chinese Medicine formula for the treatment of headache. The analytes and internal standard (IS) were separated on a SHIM‐PACK XR‐ODS II column, and the detection was performed on a UFLC‐MS/MS system with turbo ion spray source. The lower limits of quantification were 1.5, 0.5, 1.0, 2.0, 2.0, 1.0, 0.5 and 0.2 ng ml?1 for evodiamine, rutaecarpine, dehydroevodiamine, limonin, gensenoside Rb1, Rd, Re and Rg1, respectively. Linearity, accuracy, precision and absolute recoveries of the eight analytes were all within satisfaction. The IS‐normalized matrix factor was adopted for assessing the matrix effect and accompanied with a satisfactory result. The validated method has been successfully applied to compare pharmacokinetic profiles of the eight active ingredients in rat plasma between normal and headache rats after administration. Exact pharmaceutical effect of WZY decoction on headache was demonstrated by the ethological response of headache rats induced by nitric oxide donor after administration. The results indicated that the absorption of evodiamine, rutaecarpine, gensenoside Rb1, Re and Rg1 in headache group were significantly higher than those in normal group with similar concentration–time curves while no significant differences existed in limonin and ginsenoside Rd between the two groups. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

18.
A type of organic–inorganic hybrid material layered crystalline AlSPP (AlSPP) was prepared under simple conditions, completely different to the traditional hydrothermal methods, by the reaction of oligo‐styrenyl phosphonic acid with aluminum acetate and sodium dihydrogen phosphate. The microstructure of AlSPP was characterized by X‐ray diffraction, FT‐IR, atomic absorption spectroscopy, N2 volumetric adsorption, atomic force microscopy, scanning electron microscopy, transmission electron microscopy and thermogravimetric analysis. Based on the experimental date, the ideal structure model of AlSPP is proposed, which indicated that the layered crystalline AlSPP samples are special lamellar structure with many cavums, holes, channels and ravines on the surface, the interlamellar region and interlayer surfaces of the particles. Therefore AlSPP possesses excellent properties and has potential applications for heterogeneous asymmetric catalyst supports. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

19.
Electron delocalization of new mixed‐valent (MV) systems with the aid of lateral metal chelation is reported. 2,2′‐Bipyridine (bpy) derivatives with one or two appended di‐p‐anisylamino groups on the 5,5′‐positions and a coordinated [Ru(bpy)2] (bpy=2,2′‐bipyridine), [Re(CO)3Cl], or [Ir(ppy)2] (ppy=2‐phenylpyridine) component were prepared. The single‐crystal molecular structure of the bis‐amine ligand without metal chelation is presented. The electronic properties of these complexes were studied and compared by electrochemical and spectroscopic techniques and DFT/TDDFT calculations. Compounds with two di‐p‐anisylamino groups were oxidized by a chemical or electrochemical method and monitored by near‐infrared (NIR) absorption spectral changes. Marcus–Hush analysis of the resulting intervalence charge‐transfer transitions indicated that electron coupling of these mixed‐valent systems is enhanced by metal chelation and that the iridium complex has the largest coupling. TDDFT calculations were employed to interpret the NIR transitions of these MV systems.  相似文献   

20.
A magnetic metal‐organic framework (MOF) nanocomposite was successfully prepared by a new and green strategy through reasonable design. Magnetic MOF of Fe3O4‐NHSO3H@HKUST‐1 nanocomposite use for removal of lead ions as an environmental pollutant. The experimental results indicated that the nano adsorbent of Fe3O4‐NHSO3H@HKUST‐1 can removed lead ions under optimum operational conditions. The dosage of the nanocomposite, pH of the sample solution, and contact time were obtained to be 10 mg, 7.0, and 90 min, respectively, while the initial concentration of Pb(II) ions of 400 mg/L was used. A kinetic study indicated that a pseudo‐second‐order model agreed well with the experimental data. The isotherm experiments revealed that the Langmuir model attained better fits to the equilibrium data than the Freundlich model. The maximum adsorption capacity of the adsorbent for the removal of lead under the optimum operational conditions of pH 7.0 and temperature 25°C was found to be 384.6 mg/g. The thermodynamic parameters indicate that the adsorption of lead is spontaneous and endothermic. The magnetic MOF nanocomposite could be recovered easily and reused many times without significant loss of its nano‐adsorbent activity. The proposed method is simple, eco‐friendly, low cost, and efficient in the removal of lead ions from aqueous solutions.  相似文献   

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