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1.
A sensitive and efficient method for trace analysis of some phenolic compounds using simultaneous derivatization and air‐assisted liquid–liquid microextraction from human urine and plasma samples followed by gas chromatography–nitrogen phosphorous detection 下载免费PDF全文
Mir Ali Farajzadeh Mohammad Reza Afshar Mogaddam Ali Akbar Alizadeh Nabil 《Biomedical chromatography : BMC》2015,29(12):1921-1931
In present study, a simultaneous derivatization and air‐assisted liquid–liquid microextraction method combined with gas chromatography–nitrogen phosphorous detection has been developed for the determination of some phenolic compounds in biological samples. The analytes are derivatized and extracted simultaneously by a fast reaction with 1‐flouro‐2,4‐dinitrobenzene under mild conditions. Under optimal conditions low limits of detection in the range of 0.05–0.34 ng mL?1 are achievable. The obtained extraction recoveries are between 84 and 97% and the relative standard deviations are less than 7.2% for intraday (n = 6) and interday (n = 4) precisions. The proposed method was demonstrated to be a simple and efficient method for the analysis of phenols in biological samples. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
2.
Othman Belhadj Miled David Grosso Jacques Livage 《Journal of Physics and Chemistry of Solids》2004,65(10):1751-1755
This paper describes the synthesis and optical pH sensing properties of a pH indicator dye activated mesostructured silica coated optical fibre. The pH-sensitive dye bromothymol blue was incorporated into the mesostructure sol precursor and thin films/coatings were used for pH-sensing applications without prior removal of the surfactant. The pH sensitivity range and operating wavelength were analysed by absorption measurements on layer dip-coated on glass slides. The pH sensing properties of coated optical fibre were tested by evanescent wave method. Experiments were carried out by using a series of solutions of known pH. No leaching was observed (except at very high pH) and an excellent reversibility was obtained between pH=2 and 5. 相似文献
3.
Hua Zhang Nabil A. Amro Robert Elghanian Joseph Fragala 《Applied Surface Science》2006,253(4):1960-1963
A method, combining micro-contact printing (μCP), wet chemical etching and reactive ion etching (RIE), is reported to fabricate microstructures on Si and SiOx. Positive and negative structures were generated based on different stamps used for μCP. The reproducibility of the obtained microstructures shows the methodology reported herein could be useful in Micro-Electro-Mechanical Systems (MEMS), optical and biological sensing applications. 相似文献
4.
Eldefrawi ME Azer NL Nath N Anis NA Bangalore MS O'Connell KP Schwartz RP Wright J 《Applied biochemistry and biotechnology》2000,87(1):25-35
An automated flow fluorometer designed for kinetic binding analysis was adapted to develop a solid-phase competitive fluoroimmunoassay
for urinalysis of opiates. The solid phase consisted of polymer beads coated with commercial monoclonal antibodies (MAbs)
raised against morphine. Fluorescein-conjugated morphine (FL-MOR) was used as the fluorescein-labeled hapten. The dissociation
equilibrium constant (K
D
) for the binding of FL-MOR to the anti-MOR MAb was 0.23 nM. The binding of FL-MOR to the anti-MOR MAb reached steady state within minutes and was displaced effectively by morphine
and other opiates. Morphine-3-glucuronide (M3G), the major urinary metabolite of heroin and morphine, competed effectively
with FL-MOR in a concentration-dependent manner for binding to the antimorphine MAb and was therefore used to construct the
calibration curve. The sensitivity of the assay was 0.2 ng/mL for M3G. The assay was effective at concentrations of M3G from
0.2 to 50 ng/mL, with an IC50 of 2 ng/mL. Other opiates and heroin metabolites that showed >50% crossreactivity when present at 1 μg/mL included codeine,
morphine-6-glucuronide, and oxycodone. Methadone showed very low crossreactivity (<5%), which is a benefit for testing in
patients being treated for opiate addictions. The high sensitivity of the assay and the relatively high cutoff value for positive
opiate tests allows very small sample volumes (e.g., in saliva or sweat) to be analyzed. A double-blind comparison using 205
clinical urine samples showed good agreement between this single-step competitive assay and a commercially performed enzyme
multiplied immunoassay technique for the detection of opiates and benzoylecgonine (a metabolite of cocaine). 相似文献
5.
Difficulties in carrying out the free-radical addition of trialkylsilanes (as opposed to trichlorosilane) to alkene CC bonds are partly due to telomerization competing with the radical transfer step. This can be overcome by the use of a large excess of trialkylsilane, when good yields of adduct are obtained from mono-substituted and 1,2-disubstituted alkenes. 相似文献
6.
Alfy Badie Sakla Nabil Khalil Masoud Zaki Sawiris Wagih Sadik Ebaid 《Helvetica chimica acta》1974,57(2):481-487
Aryldiazophenyl sulfides prepared from diazotised arylamines and thiophenol at controlled pH, are coupled with β-naphthol yielding the corresponding azo dye. A kinetic study of the diazo coupling reaction of p-nitrobenzenediazo phenyl sulfide with β-naphthol under various conditions revealed that the reaction is of first order kinetics with respect to the diazo phenyl sulfide, and that the rate of coupling measured colorimetrically is influenced by the hydrogen ion concentration and by the ionising power of the medium. 相似文献
7.
Chiu-Hong Lin Michael D. Ennis Robert L. Hoffman Gillian Phillips Susanne R. Haadsma-Svensson Nabil B. Ghazal Connie G. Chidester 《Journal of heterocyclic chemistry》1994,31(1):129-139
An efficient synthesis of the potent and orally active 5-HT1A agonists, (R)-(+)- and (S)-(-)-1-formyl-6,7,8,9-tetrahydro-N,N-dipropyl-3H-benz[e]indol-8-amines 1a and 1b , is described. This synthesis was accomplished in twelve steps from commercially available 1,5,6,7-tetrahydro-4H-indol-4-one ( 5 ). The key step involved a regio-controlled Friedel-Crafts acylation of 1-(p-toluenesulfonyl)indol-4-acetyl chloride with ethylene to yield a versatile synthon, 3-(p-toluenesulfonyl)-6,7,8,9-tetrahydro-3H-benz[e]indol-8-one ( 10 ). Subsequent coupling of this ketone with chiral α-methylbenzylamine under reductive amination conditions yielded a mixture of diastereomers. These diastereomers were efficiently separated by either chromatography or fractional recrystallization of the derived hydrochloride salts. Debenzylation of the pure diastereomers was followed by alkylation and formylation to yield (R)-(+)- and (S)-(-)-enantiomers 1a and 1b with >99% purity. 相似文献
8.
The sensitivity of an enzyme to its environment has provoked much interest both for its immediate relevance to biochemistry and for the use of enzymes in chemical synthesis. The intercellular or extracellular environment in which an enzyme naturally operates is crowded with macromolecular, small-molecule, and ionic solutes and hence is markedly different from the dilute aqueous buffer solutions commonly cited for comparisons of biochemical processes. We report the results of a kinetic study into the effects of such a crowded solution on the rate of an enzyme-mediated process-the trypsin-catalyzed hydrolysis of a nonnatural substrate ester. The catalytic rate constant decreases linearly with solvent polarity, but substrate binding is independent of the concentration of added crowding agent up to 395 g/L. 相似文献
9.
Awadallah Adel M. El-Halabi Nabil M. Ferwanah Abdel-Rahman S. Awad Boshra M. 《Transition Metal Chemistry》2004,29(3):280-283
3-Acetyl-1,2,4-triazole hydrazones (3b,c) and methylhydrazone (4d) were prepared by reacting triazoles (1b–d) with an excess of hydrazines at room temperature. Square planar nickel(II) complexes (8b,c) of (3b,c) were obtained from their reaction with Ni(OAc)2 in a 2:1 mol ratio in EtOH at room temperature. The spectral data suggest structures (8b,c) for the obtained complexes, which result from ring opening of the triazole ring followed by recyclization to give the 5-arylhydrazono-2,3-dihydro-4H-1,2,4-triazine ligand (7b,c). The reaction of triazole methylhydrazone (4d) with Ni(OAc)2 in EtOH resulted, however, in the formation of the starting triazole (1d). All new compounds were characterized by elemental analysis, i.r., 1H-n.m.r. 13C-n.m.r. and hrms. 相似文献
10.
A simple colorimetric method for the assay of penicillin G salt and penicillamine by oxidation with iodate 总被引:1,自引:0,他引:1
A simple colorimetric procedure is described for determination of penicillin G salt and penicillamine. It is based on oxidation with potassium iodate at room temperature and measurement of the liberated iodine at 520 nm after extraction with carbon tetrachloride. Compared with other procedures, this method proved to be more rapid, highly reproducible and reasonably accurate. The relative standard deviation did not exceed 0.9% and 0.4% for penicillin and penicillamine, respectively. The procedure has been successfully applied to pharmaceutical preparations containing either of the two compounds. 相似文献