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131.
A laser induced breakdown spectrometry hyphenated with on-line continuous flow hydride generation sample introduction system, HG-LIBS, has been used for the determination of arsenic, antimony, lead and germanium in aqueous environments. Optimum chemical and instrumental parameters governing chemical hydride generation, laser plasma formation and detection were investigated for each element under argon and nitrogen atmosphere. Arsenic, antimony and germanium have presented strong enhancement in signal strength under argon atmosphere while lead has shown no sensitivity to ambient gas type. Detection limits of 1.1 mg L−1, 1.0 mg L−1, 1.3 mg L−1 and 0.2 mg L−1 were obtained for As, Sb, Pb and Ge, respectively. Up to 77 times enhancement in detection limit of Pb were obtained, compared to the result obtained from the direct analysis of liquids by LIBS. Applicability of the technique to real water samples was tested through spiking experiments and recoveries higher than 80% were obtained. Results demonstrate that, HG-LIBS approach is suitable for quantitative analysis of toxic elements and sufficiently fast for real time continuous monitoring in aqueous environments. 相似文献
132.
Ayşegül Doğan Emirhan Nemutlu M. Aykut Özek Hakan Eroğlu Sedef Kır M. Sinan Beksaç 《Chromatographia》2013,76(21-22):1513-1519
Pregnancy alters pharmacokinetic profile of many drugs, because of altering body volume and metabolism rate. Therefore, dosage rates and concentrations of drugs must be controlled during pregnancy. Here, we identified the pharmacokinetic profile of pre-operatively given cefepime in caesarean section and gynecological operations using a simple, rapid, cost-effective and valid liquid chromatographic method. The chromatographic separation was performed using 40 mM, pH 3.2 phosphate buffer containing 6 % methanol as mobile phase at 0.30 mL min?1 flow rate. Gradient elution with methanol was applied to get shorter analysis time without any interference from plasma endogens. During analyses, temperature of column, autosampler and detector were set as 30, 10 and 40 °C, respectively. The detection wavelength was 260 nm and ceftizoxime was used as internal standard. At the optimum conditions, the cefepime analysis from plasma samples was completed in 7 min. Cefepime was extracted from plasma samples using perchloric acid with a very high recovery rate (99.3 %). The method was fully validated according to the Food and Drug Administration guidelines for bioanalytical method validation, and found to be selective, linear, repeatable, reproducible and robust. After validation studies, the method was applied to five caesarean-sectioned and four non-pregnant sectioned women treated with pre-operative, prophylactic single intravenous dose of cefepime (1 g Maxipime®) in order to determine pharmacokinetic profile of cefepime. Peak serum concentrations of cefepime in caesarean-sectioned women at the arterial port after infusion was 70.11 ± 10.74 μg mL?1. The mean elimination half-life, volume of distribution and calculated area under the concentration–time curve (AUC)0–∞ were 1.10 ± 0.23 h, 14.22 ± 2.29 L and 101.55 ± 10.99 μg h mL?1 for caesarean-sectioned women; and 1.14 ± 0.21 h, 14.76 ± 2.92 L and 104.71 ± 36.34 μg h mL?1 for non-pregnant sectioned women, respectively. The area under curve, elimination half-life, maximum plasma concentration and the mean distribution volume of cefepime were not changed in case of pregnancy. 相似文献
133.
Seven [2.2.1] bridged alkenes were cleaved to the corresponding dialdehyde products by neutral heterogenous oxidation with KMnO4-CuSO4.5H2O. While endo, endo-dimethyl bicyclo[2.2.2]oct-5-ene-2,3-dicarboxylate, [2.2.2] bridged alkene, gave the corresponding α-hydroxy ketone, endo, endo-dimethyl bicyclo[3.2.2]non-8-ene-6,7-dicarboxylate afforded a diketone product. 相似文献
134.
N-Aryl-N,N-diphenacylamine dioximes were prepared by the reaction of corresponding arylamines with α-bromoacetophenone oxime in ethanol-water at room temperature. These compounds reacted with aryl isocyanates in acetonitrile to give imidazooxadiazolones 9. The probable mechanism of the reaction is discussed. 相似文献
135.
Murat Güney Selçuk Eşsiz Arif Daştan Metin Balci Ottorino De Lucchi Ertan Şahin Fabrizio Fabris 《Helvetica chimica acta》2013,96(5):941-950
Stereoisomerically pure endo‐ and exo‐7‐halo‐7‐(trimethylstannyl)benzonorcar‐3‐enes (=endo‐ and exo‐(1‐halo‐1a,2,7,7a‐tetrahydro‐1H‐cyclopropa[b]naphthalen‐1‐yl)trimethylstannane) 4 and 6 were selectively obtained by lithium? tin or magnesium? tin transmetalation in good yields (Scheme 2 and 3). The reaction of these compounds with copper(I) thiophene‐2‐carboxylate (CuTC) produced in both cases the corresponding CS‐symmetric bicyclopropylidene (=cyclopropylidenecyclopropane) syn‐ 1 , a single diastereoisomer (Schemes 5 and 6). The structure of syn‐ 1 was undoubtedly elucidated by X‐ray single crystal diffraction. The coupling mechanism of the carbenoid cyclopropane is discussed (Scheme 7). 相似文献
136.
Serkan Yavuz Hamdi Özkan Gülçin Tok Ali Dişli 《Journal of heterocyclic chemistry》2013,50(6):1437-1440
The substituted pyrolidine derivatives with high stereoselectivity were obtained through cycloaddition reaction in the presence of a Lewis acid namely diethylzinc by solvent‐free grinding method. 相似文献
137.
Aryl Grignard reagents react with N,N‐dimethyl O‐(mesitylenesulfonyl)hydroxylamine in THF under Barbier conditions at room temperature and give N,N‐dimethylanilines with high yields in a 2‐h reaction. The amination yield of in situ Grignard reagents were not lower than those of preformed aryl Grignard reagents. In situ cycloalkyl‐, allyl‐, and benzylmagnesium bromides did not react with N,N‐dimethyl O‐(mesitylenesulfonyl)hydroxylamine, except that amination of in situ n‐hexylmagnesium bromide resulted in a medium yield. Grignard–Barbier‐type amination of aryl bromides with N,N‐dimethyl O‐(mesitylenesulfonyl)hydroxylamine provides a new alternative route for the synthesis of N,N‐dimethylanilines. 相似文献
138.
Gülşah Kalaycı Murat Belivermiş Önder Kılıç Sayhan Topcuoğlu Yavuz Çotuk 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(1):239-244
This study was carried out to better understand the biokinetics of radiocesium in clams living in sediment. The accumulation and depuration kinetics of 134Cs were investigated in the Manila clam (Ruditapes philippinarum) under controlled laboratory conditions. The concentration factor was found to be 3.0 for 134Cs in the whole body; however, the concentration factor in the soft part of the clams (12) was significantly higher than those in the whole body and shell (0.80). The depuration kinetics of the radionuclide were described by a two-component exponential model for the whole body. The biological half-lives in the fast and slow components were found to be 0.63 and 22.1 days, respectively. The depuration kinetics for 134Cs in the soft parts were described by a single-component exponential model with a resultant the biological half-life of 18.0 days. 相似文献
139.
Ayşegül Kahraman Gökay Kaynak Gizem Akkaya Orhan Gürler Sezai Yalçın 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(2):1057-1066
Activity concentrations of gross-β, naturally occurring 226Ra, 232Th, 210Pb, 7Be and anthropogenic 137Cs in epiphytic lichens collected from Uluda? Mountain are presented and discussed with the aim of evaluating potential usability of lichens as a biomonitor. The activity concentrations of gross-β, 137Cs, 40K, 226Ra, 232Th, 210Pb and 7Be in the lichen samples were found to be in the range of 177–707, 4.05–94.26, 86–211, below detection limit (BDL)—19.2, BDL—14.0, 229–872, and 72.1–220.7 Bq kg?1 in dry weight, respectively. 137Cs content in collected epiphytic lichens was in descending order: Parmelia sulcata > Lobaria pulmonaria > Pseudevernia furfuracea > Usnea filipendula. The best biomonitor for 137Cs among the lichen species used in this study was determined as Parmelia sulcata. Pearson’s correlation coefficient was calculated between 137Cs and 40K activity concentrations using a statistical package program (SPSS ver. 17.0) and a negative correlation value (R = ?0,323, p = 0,222) was obtained. The highest 226Ra and 232Th activity concentrations were found in Bo?azova Yaylas? which has a geological structure including granitic rocks. It was found that 137Cs and 7Be activity concentrations in species demonstrated an inverse behaviour. The effect of mean annual precipitation and temperature on 7Be activity concentration was determined using multi regression analysis. Also, correlations between the 137Cs and 7Be, and 40K and 7Be were investigated. 相似文献
140.
For practical guest–host applications, it is important to choose dyes with a high ability of orientation in the liquid crystal (LC) matrix. In this experimental work, two different azo-structured dyes (disperse yellow 3 and 7) were separately doped to each of two different nematic LCs (E7 and ZLI-1132). Their solubilities, textures, phase transition temperatures and order parameters were determined. At the second stage, single-walled carbon nanotubes (SWCNTs) in a small amount were separately added to each of these solutions, and the experiments were repeated as similar to the previous ones. The solubilities of dyes in the LC E7 were lower than those of ZLI-1132. Moreover, the highest order parameter value was attained with yellow 7 dye in ZLI-1132 nematic host. Co-use of nanoparticles (CNTs) as dopant resulted in notable increases in order parameters. These dyes and CNTs did not significantly destabilise the mesomorphic phase of nematic hosts. An appreciable change in textures was not monitored with addition of dopant(s). In addition, it was observed that the narrowing on the temperature range of the LC did not take place with the addition of dopants to the crystal; on the contrary, an increase was recorded. 相似文献