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991.
Rosenani A. Haque Abbas Washeel Salman Srinivasa Budagumpi Amirul Al‐Ashraf Abdullah Zena A. Abdul Hameed Al‐Mudaris Amin M. S. Abdul Majid 《应用有机金属化学》2013,27(8):465-473
A series of Ag(I) complexes ( 6 , 7 , 8 , 9 ) derived from imidazol‐2‐ylidenes was synthesized by reacting Ag2O with an o‐, m‐, p‐xylyl or 1,3,5‐triazine‐linked imidazolium salts ( 1 , 2 , 3 , 4 ) and then characterizing these using various spectro‐analytical techniques. Additionally, triazine‐linked bis‐imidazolium salt 5 was characterized using the single‐crystal X‐ray diffraction method. Complexes 6–9 were formed from the N‐heterocyclic carbene ligand precursors 1–3 as PF6‐ salts in good yields. Conversely, salt 5 does not form Ag(I) complex even under various reaction conditions. Using ampicillin as a standard, complexes 6–9 were tested against bacteria strains Escherichia coli and Staphylococcus aureus as Gram‐negative and Gram‐positive bacteria, respectively, showing potent antimicrobial activities against the tested bacteria even at minimum inhibition concentration and bacterial concentration levels. Furthermore, the potential anticancer activities of the reported complexes were evaluated against the human colorectal cancer (HCT 116) cell lines, using 5‐fluorouracil as a standard drug. The highest anticancer activities were observed for complex 8 with an IC50 value of 3.4 μm , whereas the lowest was observed for complex 9 with an IC50 value of 18.1 μm . Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
992.
Yang‐Chu Lin Kung‐Lung Cheng Woan‐Shiow Tzeng Chih‐Lin Su Long‐Je Lee Ling‐Yung Wang 《Liquid crystals》2013,40(3):289-293
A series of N,N‐disubstituted‐4‐[(4‐aminophenyl)diazenyl]benzylidene‐4′‐alkylanilines (azo dyes) were synthesized from the reaction of the corresponding benzaldehyde with alkylanilines. These azo dyes exhibit nematic and SmC phases on heating. Their order parameter, photo‐stability and miscibility were studied by investigation of a representative sample. 相似文献
993.
Dai Li‐Bo Yan Miao Li Huan‐De Fang Ping‐Fei Wang Feng Deng Yang 《Biomedical chromatography : BMC》2013,27(9):1143-1149
A simple and sensitive analytical method based on ultraperformance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) has been developed for determination of moclobemide in human brain cell monolayer as an in vitro model of blood–brain barrier. Brucine was employed as the internal standard. Moclobemide and internal standard were extracted from cell supernatant by ethyl acetate after alkalinizing with sodium hydroxide. The UPLC separation was performed on an Acquity UPLCTM BEH C18 column (50 × 2.1 mm, 1.7 µm, Waters, USA) with a mobile phase consisting of methanol–water (29.5:70.5, v/v); the water in the mobile phase contained 0.05% ammonium acetate and 0.1% formic acid. Detection of the analytes was achieved using positive ion electrospray via multiple reaction monitoring mode. The mass transitions were m/z 269.16 → 182.01 for moclobemide and m/z 395.24 → 324.15 for brucine. The extraction recovery was 83.0–83.4% and the lower limit of quantitation (LLOQ) was 1.0 ng/mL for moclobemide. The method was validated from LLOQ to 1980 ng/mL with a coefficient of determination greater than 0.999. Intra‐ and inter‐day accuracies of the method at three concentrations ranged from 89.1 to 100.9% for moclobemide with precision of 1.1–9.6%. This validated method was successfully applied to bidirectional transport study of moclobemide blood–brain barrier permeability. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
994.
A selective and sensitive liquid chromatography tandem mass spectrometry method (LC‐MS/MS) was developed and validated for the determination of cefdinir in rat plasma and urine. Following a simple protein precipitation using methanol, chromatographic separation was achieved with a run time of 10 min using a Synergi 4 µ polar‐RP 80A column (150 × 2.0 mm, 4 µm) with a mobile phase consisting of 0.1% formic acid in water and methanol (65:35, v/v) at a flow rate of 0.2 mL/min. The protonated precursor and product ion transitions for cefdinir (m/z 396.1 → 227.2) and cefadroxil, an internal standard (m/z 364.2 → 208.0) were monitored in the multiple reaction monitoring in positive ion mode. The calibration curves for plasma and urine were linear over the concentration range 10–10,000 ng/mL. The lower limit of quantification was 10 ng/mL. All accuracy values were between 95.1 and 113.0% and the intra‐ and inter‐day precisions were <13.0% relative standard deviation. The stability under various conditions in rat plasma and urine was also found to be acceptable at three concentrations. The developed method was applied successfully to the pharmacokinetic study of cefdinir after oral and intravenous administration. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
995.
Silica obtained by acid treatment of sepiolite was used as a support for catalysts consisting of palladium complexes of 2‐ and 3‐thiophenecarbaldehyde. The support and the catalysts were characterized by X‐ray diffraction, and solid‐state 29Si and 13C nuclear magnetic resonance spectroscopies. The supported palladium catalysts were used in the Suzuki reaction of bromobenzene with phenylboronic acid. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
996.
Jung‐woo Chae Hyun‐moon Baek Sang Kyum Kim Ho‐il Kang Kwang‐il Kwon 《Biomedical chromatography : BMC》2013,27(8):953-955
The major metabolite of duloxetine is a glucuronide conjugate of 4‐hydroxy duloxetine (4‐HD). However, interestingly, there have been no reports determining concentrations of 4‐HD and no fully validated method has been established for measuring duloxetine and 4‐HD in rat plasma. We developed a method for the simultaneous quantification of duloxetine and its metabolite in rat plasma using high‐performance liquid chromatography tandem mass spectrometry. Duloxetine and 4‐HD were analyzed on a reverse‐phase C18 analytical column after protein precipitation of the plasma sample with methanol, using carbamazepine as an internal standard. The isocratic mobile phase of 5 mm ammonium acetate–methanol (4:6, v/v) was eluted at 0.4 mL/min. Quantification was performed on a triple‐quadrupole mass spectrometer using electrospray ionization, and the ion transition monitored in selective reaction monitoring mode. The coefficient of variation for assay precision was <18.0%, and the accuracy was 84.0–118.0%. This method was successfully used to measure the concentrations of duloxetine and its metabolite in plasma following the oral administration of a single 40 mg/kg dose in rats. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
997.
Quanfei Zou Yuan Gu Rong Lu Tiejun Zhang Guang‐Rong Zhao Changxiao Liu Duanyun Si 《Biomedical chromatography : BMC》2013,27(9):1123-1128
In this study, a simple and sensitive LC/MS/MS method was developed and validated for the determination of arctigenin in rat plasma. The MS detection was performed using multiple reaction monitoring at the transitions of m/z 373.2 → 137.3 for arctigenin and m/z 187.1 → 131.0 for psoralen (internal standard) with a Turbo IonSpray electrospray in positive mode. The calibration curves fitted a good linear relationship over the concentration range of 0.2–500 ng/mL. It was found that arctigenin is not stable enough at both room temperature and ?80 °C unless mixed with methanol before storage. The validated LC/MS/MS method was successfully applied for the pharmacokinetic study of arctigenin in rats. After intravenous injection of 0.3 mg/kg arctigenin injection to rats, the maximum concentration, half‐life and area under the concentration–time curve were 323 ± 65.2 ng/mL, 0.830 ± 0.166 and 81.0 ± 22.1 h ng/mL, respectively. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
998.
Olesya V. Zillich Ute Schweiggert‐Weisz Katrin Hasenkopf Peter Eisner Martina Kerscher 《Biomedical chromatography : BMC》2013,27(11):1444-1451
Permeation of polyphenols through the stratum corneum barrier is a precondition for the protective action of polyphenols against oxidative skin damage. Prior to in vitro skin permeation experiments, we developed a method for the quantification of polyphenols in pig skin, including organic solvent extraction and HPLC analysis. Catechine hydrate, epigallocatechin gallate, trans‐resveratrol, quercetin, rutin and protocatechuic acid were chosen for this study as representatives of phenolics with different lipophilicity and molecular weight. The antioxidative activities of polyphenols as well as their octanol–water partition coefficients at different pH values were determined. Extraction of polyphenols from pig skin was optimized by variation of solvent composition, homogenization intensity and time, as well as partial exclusion of oxygen during extraction. The highest recovery rates could be reached by extraction with the methanol–water mixture (90:10, v/v), containing 0.2 g/L l ‐ascorbic acid, after the cryo‐milling for 4 min. Recoveries of 72% for total phenolics, 96% for quercetin and protocatechuic acid, 90% for rutin and 74% for trans‐resveratrol, were achieved. These extraction parameters will be selected for the polyphenol extraction from pig skin for further in vitro drug permeation studies. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
999.
1000.