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排序方式: 共有318条查询结果,搜索用时 15 毫秒
1.
Govindarajan Sankar A. Sultan Nasar 《Journal of polymer science. Part A, Polymer chemistry》2007,45(8):1557-1570
A series of substituted N‐methylaniline‐blocked polyisocyanates based on 4,4′‐methylenebis(phenyl isocyanate) and poly(tetrahydrofuran) were prepared and characterized thoroughly with FTIR, 1H NMR, and 13C NMR spectroscopy methods. Compared with unsubstituted N‐methylaniline, a blocking agent with an electron‐releasing substituent at the para position took a shorter time, whereas those with an electron‐releasing substituent at the ortho position or an electron‐withdrawing substituent at the ortho and para positions took longer times for the blocking reaction. The thermal dissociation reactions of blocked polyisocyanates were carried out with an FTIR spectrophotometer attached to hot‐stage accessories under dynamic and isothermal conditions. The dynamic method was used to determine the deblocking temperature, and the isothermal method was used to calculate the deblocking kinetics and activation parameters. The cure times of blocked polyisocyanates with hydroxyl‐terminated polybutadiene were also determined. The deblocking temperatures, the results of cure‐time studies, and the kinetic parameters revealed that the thermal dissociation of the N‐methylaniline‐blocked polyisocyanates was retarded by electron‐donating substituents and facilitated by electron‐withdrawing substituents. The action of N‐methylanilines as blocking agents for isocyanate was explained by the formation of a four‐center, intramolecularly hydrogen‐bonded ring structure during the thermal dissociation of the blocked polyisocyanates. The formation of such a hydrogen‐bonded ring structure was confirmed and supported by variable‐temperature 1H NMR studies and entropy parameters, respectively. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 1557–1570, 2007 相似文献
2.
The synthesis of a new endo-calix[4]naphthalene is described. The reaction sequence involves the cyclocondensation of a key bisnaphthylmethane intermediate (8) with formaldehyde. This key intermediate (8) is formed using a modified Suzuki-Miyaura Pd-catalyzed cross-coupling reaction between bromomethylnaphthyl (6) and naphthylboronic acid (7), both of which can be derived from 2-hydroxynaphthoic acid. 相似文献
3.
A new simple flow injection spectrophotometric method for the assay of chlorpromazine using cerium(IV) in sulfuric acid media was developed. The oxidized form of the drug was monitored at the maximum absorbance of 526 nm. The optimum conditions were 0.035M sulfuric acid, 3.80 x 10(-3)M cerium(IV), flow rate 4.85 ml/min, coil length 45 cm and sample size 110 mm(3). Optimization was carried out by the modified simplex method. Response surface methodology was employed to investigate the ruggedness of the method. A sampling frequency of 120 hr(-1) was attained. Relative standard deviations for standard sample were usually less than 0.75. The method was applied to the determination of chlorpromazine in proprietary drugs and results were statistically compared with the official British Pharmacopoeia (BP) method. 相似文献
4.
A reasonably sensitive and highly selective spectrophotometric method for the determination of mercury(II) is proposed. The method is based on the extraction of the ion-associate formed by a mercury(II) thiacrown ether cationic complex with Bromocresol Green as the anionic counter-ion using chloroform as the extracting solvent. The effect of thiacrown ethers of different cavity sizes, namely 1,4,7,10,13-pentathiacyclopentadecane (PTP) and 1,4,7,10,13,16-hexathiacyclooctadecane (HTO), the thiacrown ether concentration, the extracting solvent, the bromocresol green concentration and the aqueous phase pH on the extraction were investigated. Measurement of the absorbance at the lambda(max) (420 nm) of the extracted ion-associate reveals that Beer's law is obeyed over 0.5-12.0 ppm mercury(II) for both ligands. Slight interference from copper(II) and cadmium(II) is exhibited by the PTP ligand, while HTO is negligibly affected by these metal ions. Strong interference from silver(I) is evident for both ligands while alkali, alkaline earth and other transition metals tested posed negligible interference. Analysis of mercury in synthetic complex mixtures was satisfactory. 相似文献
5.
Ahmed I. Foudah Sultan Alshehri Faiyaz Shakeel Mohammed H. Alqarni Tariq M. Aljarba Prawez Alam 《Molecules (Basel, Switzerland)》2022,27(13)
The study aimed to develop a new reverse-phase high-performance liquid chromatography (RP-HPLC) method with diode array detection (DAD) detection for simultaneous estimation of escitalopram (EST) and clonazepam (CZP) in tablet dosage forms with a quality by design (QbD) approach. The chromatographic conditions were optimized by Box-Behnken design (BBD) and developed method was validated for the linearity, system suitability, accuracy, precision, robustness, sensitivity, and solution stability according to International Council for Harmonization (ICH) guidelines. EST and CZP standard drugs peaks were separated at retention times of 2.668 and 5.046 min by C-18 column with dimension of 4.6 × 100 mm length and particle size packing 2.5 µm. The mobile phase was methanol: 0.1% orthophosphoric acid (OPA) (25:75, v/v), with a flow rate of 0.7 mL/min at temperature of 26 °C. The sample volume injected was 20 µL and peaks were detected at 239 nm. Using the standard calibration curve, the % assay of marketed tablet was founded 98.89 and 98.76 for EST and CZP, respectively. The proposed RP-HPLC method was able to detect EST and CZP in the presence of their degradation products, indicating the stability-indicating property of the developed RP-HPLC method. The validation parameter’s results in terms of linearity, system suitability, accuracy, precision, robustness, sensitivity, and solution stability were in an acceptable range as per the ICH guidelines. The newly developed RP-HPLC method with QbD application is simple, accurate, time-saving, and economic. 相似文献
6.
Noha M. Soliman Faiyaz Shakeel Nazrul Haq Fars K. Alanazi Sultan Alshehri Mohsen Bayomi Ahmed S. M. Alenazi Ibrahim A. Alsarra 《Molecules (Basel, Switzerland)》2022,27(14)
Various chitosan (CS)-based nanoparticles (CS-NPs) of ciprofloxacin hydrochloride (CHCl) have been investigated for therapeutic delivery and to enhance antimicrobial efficacy. However, the Box–Behnken design (BBD)-supported statistical optimization of NPs of CHCl has not been performed in the literature. As a result, the goal of this study was to look into the key interactions and quadratic impacts of formulation variables on the performance of CHCl-CS-NPs in a systematic way. To optimize CHCl-loaded CS-NPs generated by the ionic gelation process, the response surface methodology (RSM) was used. The BBD was used with three factors on three levels and three replicas at the central point. Tripolyphosphate, CS concentrations, and ultrasonication energy were chosen as independent variables after preliminary screening. Particle size (PS), polydispersity index (PDI), zeta potential (ZP), encapsulation efficiency (EE), and in vitro release were the dependent factors (responses). Prepared NPs were found in the PS range of 198–304 nm with a ZP of 27–42 mV. EE and drug release were in the range of 23–45% and 36–61%, respectively. All of the responses were optimized at the same time using a desirability function based on Design Expert® modeling and a desirability factor of 95%. The minimum inhibitory concentration (MIC) of the improved formula against two bacterial strains, Pseudomonas aeruginosa and Staphylococcus aureus, was determined. The MIC of the optimized NPs was found to be decreased 4-fold compared with pure CHCl. The predicted and observed values for the optimized formulation were nearly identical. The BBD aided in a better understanding of the intrinsic relationship between formulation variables and responses, as well as the optimization of CHCl-loaded CS-NPs in a time- and labor-efficient manner. 相似文献
7.
新疆天山三种蕨类植物的总黄酮含量研究 总被引:4,自引:0,他引:4
对3种新疆蕨类植物总黄酮含量进行了分析和研究,发现黄酮类化合物普遍存在于蕨类植物中,不管是地上部分还是地下部分.不同蕨类植物不同部位的总黄酮含量差异显著.分析的三种蕨类植物中,磷毛蕨所含总黄酮量为1.79%,欧亚水龙骨营养叶总黄酮含量为0.9%,较低.在所测试样品的三个部位中,孢子叶的总黄酮含量较高. 相似文献
8.
Dibyalochan Mohanty Ameeduzzafar Zafar Mohammed Jafar Atul Kumar Upadhyay Mohammad Akiful Haque Jeetendra Kumar Gupta Vasudha Bakshi Mohammed M. Ghoneim Sultan Alshehri Mohammed Asadullah Jahangir Mohammed Javed Ansari 《Molecules (Basel, Switzerland)》2022,27(9)
Objective: The present study aimed to develop and optimize esomeprazole loaded proniosomes (EZL-PNs) to improve bioavailability and therapeutic efficacy. Method: EZL-PNs formulation was developed by slurry method and optimized by 33 box-Bhekhen statistical design software. Span 60 (surfactant), cholesterol, EZL concentration were taken as independent variables and their effects were evaluated on vesicle size (nm), entrapment efficiency (%, EE) and drug release (%, DR). Furthermore, optimized EZL-PNs (EZL-PNs-opt) formulation was evaluated for ex vivo permeation, pharmacokinetic and ulcer protection activity. Result: The EZL-PNs-opt formulation showed 616 ± 13.21 nm of vesicle size, and 81.21 ± 2.35% of EE. EZL-PNs-opt exhibited negative zeta potential and spherical confirmed scanning electron microscopy. EZL-PNs-opt showed sustained release of EZL (95.07 ± 2.10% in 12 h) than pure EZL dispersion. The ex-vivo gut permeation result exhibited a significantly (p < 0.05) enhanced flux than pure EZL. The in vivo results revealed 4.02-fold enhancement in bioavailability and 61.65% protection in ulcer than pure EZL dispersion (43.82%). Conclusion: Our findings revealed that EZL-PNs formulation could be an alternative delivery system of EZL to enhance oral bioavailability and antiulcer activity. 相似文献
9.
Clifton K. Fagerquist Omar Sultan Michelle Q. Carter 《Journal of the American Society for Mass Spectrometry》2012,23(12):2102-2114
We previously reported the apparent formation of matrix adducts of 3,5-dimethoxy-4-hydroxy-cinnamic acid (sinapinic acid or SA) via covalent attachment to disulfide bond-containing proteins (HdeA, Hde, and YbgS) from bacterial cell lysates ionized by matrix-assisted laser desorption/ionization (MALDI) time-of-flight-time-of-flight tandem mass spectrometry (TOF-TOF-MS/MS) and post-source decay (PSD). We also reported the absence of adduct formation when using ??-cyano-4-hydroxycinnamic acid (CHCA) matrix. Further mass spectrometric analysis of disulfide-intact and disulfide-reduced over-expressed HdeA and HdeB proteins from lysates of gene-inserted E. coli plasmids suggests covalent attachment of SA occurs not at cysteine residues but at lysine residues. In this revised hypothesis, the attachment of SA is preceded by formation of a solid phase ammonium carboxylate salt between SA and accessible lysine residues of the protein during sample preparation under acidic conditions. Laser irradiation at 355?nm of the dried sample spot results in equilibrium retrogradation followed by nucleophilic attack by the amine group of lysine at the carbonyl group of SA and subsequent amide bond formation and loss of water. The absence of CHCA adducts suggests that the electron-withdrawing effect of the ??-cyano group of this matrix may inhibit salt formation and/or amide bond formation. This revised hypothesis is supported by dissociative loss of SA (?224?Da) and the amide-bound SA (?206?Da) from SA-adducted HdeA and HdeB ions by MS/MS (PSD). It is proposed that cleavage of the amide-bound SA from the lysine side-chain occurs via rearrangement involving a pentacyclic transition state followed by hydrogen abstraction/migration and loss of 3-(4-hydroxy-3,5-dimethoxyphenyl)prop-2-ynal (?206?Da). 相似文献
10.