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1.
Yi Zheng Ziqing Wang Gabrielle Lui Dborah Hirt Jean‐Marc Treluyer Sihem Benaboud Radia Aboura Ins Gana 《Biomedical chromatography : BMC》2019,33(5)
Levofloxacin, pefloxacin, ciprofloxacin and moxifloxacin are four fluoroquinolones used in the treatment of serious bacterial infections. The antibacterial activity of fluoroquinolones is concentration dependent. Therefore, therapeutic drug monitoring in daily clinical practice is warranted to ensure the therapy's efficacy and prevent bacterial resistance. The purpose of the present study was to develop a method using high‐pressure liquid chromatography with an ultraviolet detector for simultaneous quantification of these four fluoroquinolones in human plasma. A 50 μL aliquot of plasma was precipitated by 200 μL of methanol using gatifloxacin as internal standard. The chromatographic separation was performed on a Kinetex XB‐C18 column using a mobile phase composed of a mixture of orthophosphoric acid 0.4% (v/v), acetonitrile and methanol at a flow rate of 1.2 mL/min. Dual UV wavelength mode was used, with levofloxacin and moxifloxacin monitored at 293 nm, and pefloxacin and ciprofloxacin monitored at 280 nm. The calibration was linear over the ranges of 0.125–25 mg/L for levofloxacin, 0.1–20mg/L for moxifloxacin and 0.05‐10 mg/L for both pefloxacin and ciprofloxacin. Inter‐ and intra‐day trueness and precision were <13% for all the compounds under study. The proposed method was simple, reliable, cost‐effective and suitable for therapeutic drug monitoring or pharmacokinetics studies. 相似文献
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Griesbeck AG Gudipati MS Hirt J Lex J Oelgemoller M Schmickler H Schouren F 《The Journal of organic chemistry》2000,65(21):7151-7157
The regioselectivity of photoinduced electron-transfer (PET) reactions of unsymmetrical phthalimides is controlled by the spin density distribution of the intermediate radical anions. ROHF ab initio calculations were found to be most suitable for atomic spin density analysis. Intramolecular PET reactions of quinolinic acid imides were studied with the potassium butyrate and hexanoate 1a,b and a cysteine derivative 3. The photocyclizations products 2a,b and 4 were formed with moderate regioselectivities (68:32, 57:43, and 81:19) showing preferential ortho cyclization. The intermolecular reaction of potassium propionate and potassium isobutyrate with N-methylquinolinic acid imide (5) yielded as addition products the dihydropyrrolo[3,4-b]pyridines 6a,b with slight ortho regioselectivity (55:45). In contrast to these low regioselectivities, the PET reaction of potassium propionate with the methyl ester of N-methyltrimellitic acid imide (9) yielded solely the para addition product 10. Likewise, the intramolecular photoreaction of the cysteine derivative 7 gave a 75:25 (para/meta) mixture of regioisomeric cyclization products 8. The regioselectivity originates from donor-acceptor interactions prior to electron transfer and differences in spin densities in the corresponding imide radical anions. The results of DFT and ab initio calculations for the radical anions of the quinolinic acid imide (11(*)(-)) and the methyl ester of trimellitic acid imide (12(*)(-))( )()were in agreement with the latter assumption: spin densities in 11(*)(-) were higher for the imido ortho carbon atoms (indicating preferential ortho coupling); for 12(*)(-) the spin densities were higher for the imido para carbon atoms (indicating preferential para coupling). These correlations became more significant when the additional spin densities at the carbonyl oxygen and the adjacent carbon atoms were taken into account. The cyclization selectivities for 2, 4, and 8 deviate from the intermolecular examples probably because of ground-state and solvent effects. 相似文献
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O. Hehner R. Warington Sutton Alfred Smetham L. Hirt Cohn A. Certes und H. Zerener 《Fresenius' Journal of Analytical Chemistry》1881,20(1):292-295
Ohne Zusammenfassung 相似文献
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RolandA. Breitenmoser ThomasR. Hirt RoelandT.N. Luykx Heinz Heimgartner 《Helvetica chimica acta》2001,84(4):972-979
The synthesis of methyl (2S,4R)‐4‐(benzyloxy)‐N‐(2,2‐dimethyl‐2H‐azirin‐3‐yl)prolinate ( 10 ), a novel 2H‐azirin‐3‐amine (`3‐amino‐2H‐azirine'), is described (Scheme 1). The reaction of methyl (2S,4R)‐N‐(2‐methylpropanoyl)‐4‐(benzyloxy)prolinate ( 7 ) with Lawesson reagent gave methyl (2S,4R)‐4‐(benzyloxy)‐N‐[2‐(methylthio)propanoyl]prolinate ( 8 ) and consecutive treatment with COCl2, 1,4‐diazabicyclo[2.2.2]octane (DABCO), and NaN3 led to 10 . The use of 10 as a building block of the dipeptide Aib‐Hyp (Aib=2‐aminoisobutyric acid, Hyp=(2S,4R)‐4‐hydroxyproline) is demonstrated by the syntheses of several model peptides (Scheme 2 and Table). The benzyl protecting group of the 4‐OH function in Hyp in the model peptides has been removed in good yields. 相似文献
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J. Geiss P. Hirt und H. Leutwyler 《Zeitschrift für Angewandte Mathematik und Physik (ZAMP)》1969,20(4):607
Ohne Zusammenfassung 相似文献
8.
Adsorption of fluorescently labeled protein residues on poly(ethylene-co-acrylic acid) films modified with affinity functionalities 总被引:1,自引:0,他引:1
Poly(ethylene-co-acrylic acid) (EAA) films were reacted with glycine, 12-aminododecanoic acid, aspartic acid, 5-aminoisophthalic acid, ethanolamine, diethylamine, dimethylamine, N-isopropylamine, and dimethylaminoethyleneamine to prepare EAA films with negatively charged, non-charged, hydrophilic, and hydrophobic functionalities. Attenuated total reflectance Fourier transform infrared spectroscopy, differential scanning calorimetry, and contact angle measurements were used to characterize the modified EAA films. Analyses revealed that the films were modified on the surfaces and also in the bulk; therefore, bulk properties such as cohesive energy density were changed even though the surfaces remained hydrophobic. Adsorption studies were performed for two fluorescently labeled protein residues, dansyl-L-phenylalanine (dansyl-F) and dansyl-L-glutamine (dansyl-Q), from pH 7.4 buffer solutions. The adsorption results revealed that dimethylaminoethyleneamine functionality gave the highest uptake among the functionalities studied, and adsorption was more favorable for dansyl-F than dansyl-Q. Adsorption behavior is discussed in terms of hydrophobic-hydrophobic (dispersion) interactions and Coulombic interactions. 相似文献
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Janorkar AV Luo N Hirt DE 《Langmuir : the ACS journal of surfaces and colloids》2004,20(17):7151-7158
Polymer films can be tailored for a specific application by modifying their surface properties. In this study, linear and branched architectures were grafted to ethylene-acrylic acid (EAA) copolymer films using the so-called grafting from approach. Dicyclohexylcarbodiimide was used to activate the carboxylic acid functionality on the surface of the EAA copolymer film before reacting it with selected di- and tri-amine compounds. The carboxylic acid functionality was subsequently regenerated by reacting the amine-grafted film with succinic anhydride. These reaction steps were then repeated to create the linear and branched architectures on the EAA film surface. The film surface resulting from each reaction step was analyzed using attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and contact angle measurements. A systematic analysis of the ATR-FTIR results was performed to estimate the average conversion of the reaction schemes and to explain the observed contact angle results. A significant reduction in water contact angle for the EAA film grafted with a branched architecture was observed. The EAA film grafted with a linear architecture showed a marginal reduction in water contact angle when ethanol was used as a solvent for ethylenediamine. When the solvent for ethylenediamine was changed to water, the contact angle decreased noticeably. However, analysis of control films showed that the reduction in the contact angles was due to the solvent treatment. In the case of branched architectures, such reduction in contact angle due to the solvent treatment was not observed. Several control experiments were performed to ensure that the reduction in the contact angles was in fact due to the grafted species and not due to exposure to various solvents used in the reaction scheme. 相似文献