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951.
Ultrasonic back-extraction of Triton X-100 reverse micelles by a water/chloroform binary system and gas chromatography with flame ionization detection (GC-FID) was developed for extraction and determination of β-sitosterol and cholesterol in soybean and sunflower oil samples. After the homogenization of the oil samples with Triton X-100, an aliquot of 200 μL of methanol was added to the samples to form two phases. The clear Triton X-100 extract obtained by centrifugation was treated with a mixture of water (1000 μL) and chloroform (300 μL) for back-extraction of the analytes into the chloroform phase by ultrasonication. After centrifugation, the sedimented chloroform layer was withdrawn easily by a microsyringe and directly injected into the GC-FID system. The influence of several important parameters on the extraction efficiencies of the analytes was evaluated. Under optimized experimental conditions, the calibration graphs were linear in the range of 1.0–30.0 mg L−1 with coefficient of determination more than 0.994 for both analytes. The method detection limit values were in the range of 0.2–0.7 mg L−1. The lower limit of quantification values were in the range of 0.7–2.4 mg L−1. Intra-day relative standard deviations were in the range of 1.0–2.7%. This procedure was successfully applied with satisfactory results to the determination of β-sitosterol and cholesterol in spiked oil samples. The relative mean recoveries of oil samples ranged from 93.6% to 105.0%. 相似文献
952.
Gold nanoparticles (AuNPs) were electrodeposited on the surface of pencil graphite (PG) by fast scan cyclic voltammetry without using any additives in acidic medium. The effect of deposition time on the size of electrodeposited AuNPs was investigated in sulfuric acid as a supporting electrolyte. The deposition time was varied by varying the scan rate, number of cycles and applied potential range. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X‐ray diffraction (XRD) were used for characterization of PG and electrodeposited AuNPs. The results confirmed that nanosized gold particles (20 ± 8 nm) were deposited on the PG substrate with almost spherical geometry. 相似文献
953.
Behrooz Alirezapour Amir Reza Jalilian Mohammad Javad Rasaee Saeed Rajabifar Kamal Yavari Mohsen Kamalidehghan Fatemeh Bolourinovin Gholamreza Aslani 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(2):1261-1271
Breast cancer radioimmunoscintigraphy targeting HER2/neu expression is a growing field of work in nuclear medicine research. Trastuzumab is a monoclonal antibody that binds with high affinity to HER2/neu, which is over expressed on breast and other tumors. Developing new tracers for the detection of this cancer is of great interest. In this study, trastuzumab was successively labeled with [64Cu]CuCl2 after conjugation with DOTA-NHS-ester. The conjugate was purified by molecular filtration, the average number of DOTA conjugated per mAb was calculated and total concentration was determined by spectrophotometric method. DOTA–trastuzumab was labeled with 64Cu produced by 68Zn(p,αn)64Cu nuclear reaction (30 MeV protons at 180 μA). Radiochemical purity, integrity of protein after radiolabeling and immunoreactivity of radiolabeled mAb trastuzumab with HER2/neu antigen and SkBr3 cell line were performed by RIA. In vitro stability of radiolabeled mAb in human serum was determined by thin layer chromatography. In vitro internalization studies were performed with the SkBr3 cell line and the tissue biodistribution of the 64Cu–DOTA–trastuzumab was evaluated in wild-type rat (90 ± 5.5 μCi, 2, 6, 12, 24 h p.i.). The radioimmunoconjugate was prepared with a radiochemical purity of higher than 96 ± 0.5 % (ITLC) and specific activity as high as 5.3 μCi/μg. The average number of chelators per antibody for the conjugate used in this study was 5.8/1. The sample was showed to have similar patterns of migration in the gel electrophoresis. The 64Cu–DOTA–trastuzumab showed high immunoreactivity towards HER2/neu antigen and SkBr3 cell line. In vitro stability of the labeled product was found to be more than 94 % in PBS and 82 ± 0.5 % in human serum over 48 h. In vitro internalization studies of the 64Cu–DOTA–trastuzumab showed that up to 11.5 % of the radioimmunoconjugate internalized after 10 h. The accumulation of the radiolabeled mAb in liver, skin, intestine, lung, spleen, kidney and other tissues demonstrates a similar pattern to the other radiolabeled anti-HER2 immunoconjugates. 64Cu–DOTA–trastuzumab is a potential compound for molecular imaging of PET for diagnosis and treatment studies and follow-up of HER2 expression in oncology. 相似文献
954.
Mahmoud Roushani Zahra Saedi Yar Mohammad Baghelani Fatemeh Hamdi 《International journal of environmental analytical chemistry》2013,93(15):1586-1603
ABSTRACTIn this paper, a novel, simple, selective and effective solid phase extraction method based on ion-imprinted polymer (IIP) technology and flame atomic absorption spectrometry (FAAS) for separation and pre-concentration of trace amounts of titanium (IV) ions was reportd?. It was obtained by precipitation polymerisation by using 2-(2,4-dihydroxyphenyl)-3,5,7-trihydroxychromen-4-one titanium (IV) complex abbrivated as Ti(IV)-(morin), as the template molecule. After polymerisation, leaching the polymer in HNO3 (50% (v/v) solution caused formation cavities in the polymer. Characterisation studies of the ?Ti(IV)-imprinted polymer (Ti-IP) was performed by FT-IR, UV-Vis and scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS) techniques and then, the effective factors on extraction were optimised. A sensitive response to Ti(IV) within a concentration range between 0.01 and 4.0 μg mL?1 was achieved under the optimum conditions. A total of 10.0 ng mL?1 and 80.0 mg g?1 were obtained as limit of detection (LOD, 3Sb/m) and maximum adsorption capacity, respectively. The relative standard deviation (RSD) for eight replicates detections of 0.2 μg mL?1 of Ti(IV)? was found to be 2.8%. By this method, pre-concentration factor (PF) of 100 was obtained. Successfully applying this method in the water and standard samples, reasonable results were obtained for the extraction and pre-concentration of the titanium ions. 相似文献
955.
Angel Rodriguez-Lafuente Fatemeh S. Mirnaghi Janusz Pawliszyn 《Analytical and bioanalytical chemistry》2013,405(30):9723-9727
The use of thin-film solid-phase microextraction (SPME) as the sampling preparation step before direct analysis in real time (DART) was evaluated for the determination of two prohibited doping substances, cocaine and methadone, in urine samples. Results showed that thin-film SPME improves the detectability of these compounds: signal-to-blank ratios of 5 (cocaine) and 13 (methadone) were obtained in the analysis of 0.5 ng/ml in human urine. Thin-film SPME also provides efficient sample cleanup, avoiding contamination of the ion source by salt residues from the urine samples. Extraction time was established in 10 min, thus providing relatively short analysis time and high throughput when combined with a 96-well shaker and coupled with DART technique. Figure
Schematic protocol for determination of cocaine and methadone in urine by thin-film SPME and DART-MS analysis 相似文献
956.
Shahla Ahmadian-Fard-Fini Masoud Salavati-Niasari Azam Monfared Fatemeh Mohandes 《Comptes Rendus Chimie》2013,16(9):778-788
Pure cubic phase lead telluride (PbTe) nanostructures have been produced by using a Schiff-base complex as a precursor in the presence of microwave irradiation. The Schiff base used as ligand was derived from salicylaldehyde and ethylenediamine. The Schiff-base complex was marked as [Pb(salen)]. In addition, the effect of the irradiation time and the type of reducing agent on the morphology and purity of the final products was investigated. The as-synthesized PbTe nanostructures were characterized extensively by techniques like X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The microwave formation mechanism of the PbTe nanostructures was studied by XRD patterns of the products. Although it was found that both ionic and atomic mechanisms could take place for the preparation of PbTe, the main steps were according to the atomic reaction process, which could occur between elemental Pb and Te. 相似文献
957.
Masoud Salavati-Niasari Hamideh Seyghalkar Omid Amiri Fatemeh Davar 《Journal of Cluster Science》2013,24(1):365-376
α-Ni(OH)2 flower-like nanostructures were successfully synthesized through one-step hydrothermal method with nickel acetate tetrahydrate, ethylene-1,2-diamine (en), hexamethylenetetramine (HMT) and cetyltrimethylammonium bromide (CTAB) as morphology-directing agents. Optimum conditions to obtain high yield and pure phase α-Ni(OH)2 were identified by varying experimental parameters such as: en, HMT and CTAB concentration and reaction temperature. The products were characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared and thermogravimetric analysis. These results indicated that the α-nickel hydroxide contains water molecules and anions. The hierarchical NiO nanostructures were obtained by the as-synthesized α-Ni(OH)2 nanostructures annealed at 300 °C for 4 h. 相似文献
958.
Fatemeh F. Bamoharram Mina Roshani Majid M. Heravi Shahla Safaie 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2833-2841
Under mild conditions, monosubstituted benzyl alcohols were oxidized to benzaldehydes and benzoic acids in the presence of sodium 30-tungstopentaphosphate (Preyssler's anion), [NaP5W30O120]14? , and hydrogen peroxide as an oxidant. This polyanion with high hydrolytic stability (pH = 0–12), high thermal stability, and high acidic strength shows good activities. The effects of various parameters on the yield of the products, including a catalyst type, a nature of the substitutents, and temperature, were studied. Comparison between Keggin's heteropolyacids, H3[PW12O40], H3[PMo12O40], H4[SiW12O40], and H4[SiMo12O40], and Preyssler's anion shows that this polyanion reacts similar to Keggin's acids whitout any degradation of the structure. 相似文献
959.
Azam Farshadi Ali Ramazani Amir Tofangchi Mahyari Mehdi Khoobi Yavar Ahmadi Fatemeh Zeinali Nasrabadi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2489-2495
Protonation of the highly reactive 1:1 intermediates, produced in the reaction between triphenylphosphine and alkyl acetylenecarboxylates (or ethyl 3-phenyl-2-propynoate), by azathioprine or imidazole leads to vinyltriphenylphosphonium salts, which undergo a Michael addition reaction with a conjugate base to produce phosphorus ylides. Dipotassium hydrogen phosphate, potassium dihydrogen phosphate, and potassium iodide were found to catalyze the conversion of the phosphorus ylides to electron-poor N-vinyl imidazoles in solvent-free conditions under thermal (90°C, 1 h) conditions. The structural analysis of the products indicated that the reaction is regio- and stereoselective. 相似文献
960.
Abdolhamid Bamoniri Arash Ghorbani-Choghamarani Bi Bi Fatemeh Mirjalili 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):381-388
Abstract A wide range of aromatic aldehydes has been selectively converted to 1,1-diacetates using silica chromate (SiO2?O?CrO2?O?SiO2) under solvent-free conditions at room temperature in moderate to good yields. This protocol is mild and efficient compared to other reported methods. GRAPHICAL ABSTRACT 相似文献