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61.
Summary A method was devised to assay four forms of vitamin C: L-ascorbic acid (AA), dehydroascorbic acid (DHA), ascorbate-2-mono-
and polyphosphate (AMP, APP), as well as ascorbate-2-monosulphate (AMS), in sample series of different fish tissues and feed.
Direct and indirect detection were combined. Sample extractions were carried out with 0.2 mol L−1 sodium acetate buffer (pH 4.8) and extracts were deproteinized after different chemical or enzymatic reactions, with perchloric
acid. The DHA was reduced to AA with dithioerythritol (DTE). Ascorbate oxidase enzyme was used for the detection of background
and an acidic phosphatase enzyme for the hydrolysis of different phosphate esters. Ascorbate-2-sulphate was detected directly
with help of coinjection of the compound. Chromatographic analysis was carried out with a single column isocratic reverse
phase method. The mobile phase was an aqueous buffer of 0.04 M sodium-acetate, 0.05 mM EDTA, 0.5 mM tetrabutylammonium dihydrogen
phosphate (TBA) adjusted to pH 3.76 with 85% H3PO4 and with 24 mL methanol added to 1000 mL. C-18 columns were used with 0.6 mL min−1 flow rate at 23°C. The vitamin C forms were detected by UV absorption at 250 nm. The determination limit was 1.0–5.0 μg g−1 in AA equivalent. The standard deviations were between 1–6% and depended on the concentrations of vitamin C forms and tissues.
Recoveries were between 90–96% in samples.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997 相似文献
62.
X. Andrew Guo Allen D. Hunter Jie Chen 《Journal of polymer science. Part A, Polymer chemistry》1994,32(1):47-56
Five acrylic esters having different fluorine contents and distributions in their side-groups (i.e., CH2=CHC(O)OR, where R = ? C(CH3)2C6F4H, ? C(CH3)2C6F5, ? C(CF3)2C6F5, ? C(CF3)2C6H5, and ? C(CH3)2C6H5) have been prepared from the reactions of the lithium salts of their corresponding alcohols with acryloyl chloride. These monomers are polymerized under identical conditions by the radical initiator AIBN and five polyacrylates were prepared having the structure of ? [ ? CH2CHC(O)OR? ]n? . These addition polymers were compared and fully characterized by GPC, VPO, DSC, TGA, NMR, IR, and UV-visible spectroscopies, and they showed potential for practical applications. Significant differences in their thermal stabilities were found with respect to fluorine contents and distributions in these polyacrylates, and the highest stability arises from CF3 substitutions in the side-chains of the polymers. © 1994 John Wiley & Sons, Inc. 相似文献
63.
I. V. Ukrainets N. L. Bereznyakova G. P. Petyunin I. A. Tugaibei V. B. Rybakov V. V. Chernyshev A. V. Turov 《Chemistry of Heterocyclic Compounds》2007,43(6):729-739
An improved method for the preparation and purification of ethyl 2-hydroxy-4-oxo-4H-pyrido[1,2-a]-pyrimidine-3-carboxylates
is proposed. According to 1H and 13C NMR spectroscopic data the synthesized compounds exist in DMSO solution in the 2-hydroxy-4-oxo form while in the crystal
(at least for the case of the unsubstituted derivative) X-ray analysis shows that it occurs in the bipolar 2,4-dioxo form.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 864–876, June, 2007. 相似文献
64.
Yun-Yun Yang 《Tetrahedron》2006,62(43):10079-10086
A Zn(OTf)2-catalyzed cascade reaction of anilines with aromatic aldehydes and carbonyl compounds was described. This one-pot three-component reaction afforded the corresponding β-amino carbonyl compounds, β-amino esters, and β-amino ketones in good to excellent yields. The reaction was also applied for the liquid-phase synthesis of β-amino carbonyl compound library using PEG as a support. 相似文献
65.
Gas chromatography-mass spectrometry was applied to the cyclohexane extract of Curcuma longa L. The chromatographic conditions generated retention indices very close i.e., greater than 99.9%, to those reported for structures in the Sadtler Standard Gas Chromatography Retention Index Library. In addition to the extensively reported sesquiterpene ketones, this essential oil extract contained a series of saturated and unsaturated fatty acids. Wiley mass spectra library matching for the free fatty acids, their trimethylsilyl esters and methyl esters narrowed their identity down to a few candidates. Combining this information with the retention indices of the fatty acid methyl esters in the Sadtler library allowed the identification of some of the double bond positions. 相似文献
66.
Zusammenfassung Die Synthese der Titelverbindungen3 (R
1=R
2=C2H5;n-C4H9) durch Reaktionen von N-(N,N-Diethylthiocarbamoyl)-benzimidoylchlorid (2) mit Natriumdialkyldithiocarbamaten (1) in Aceton wird beschrieben. Die niedrigen Ausbeuten (bis 25% d.Th.) sind durch Nebenreaktionen bedingt. Die Strukturen der Verbindungen werden durch IR-,1H-NMR-,13C-NMR-und Massenspektren bestätigt. Nebenreaktionen werden13C-NMR-spektroskopisch verfolgt und die Ergebnisse diskutiert.
S-(N-(thiocarbamoyl)benzimido)dithiocarbamic esters
Summary The synthesis of the title compounds3 (R 1=R 2=C2H5;n-C4H9) by reactions of N-(N,N-diethylthiocarbamoyl)benzimidechloride (2) with sodiumdialkyldithiocarbamates (1) in acetone is described. The low yields (<25%) are caused by the occurrence of side reactions. The structures of the compounds were confirmed by IR,1H and13C NMR, and mass spectroscopy. Side reactions were detected by13C NMR spectroscopy; the results are discussed.相似文献
67.
Esters of (arylhydrazono)chloroacetic acid reacted with tris(hydroxymethyl)aminomethane in the presence of trimethylamine under mild conditions to give 3-(arylhydrazonoyl)-5,5-di(hydroxymethyl)-2-oxomorpholines. 相似文献
68.
A new preparative route for silyl esters is described, involving reaction of silyl bromide and trisalkyltin esters. The far infrared spectrum of some simple esters are reported; an investigation of the shifts in the carbonyl stretching band on condensation shows no significant differences in behaviour between methyl and silyl esters.
Darstellung einiger Silylester und Untersuchung der Vibrationsspektren in der Gasphase und in kondensierter Phase
Zusammenfassung Es wird ein neuer präparativer Weg (über Silylbromid und Trisalkylzinnester) für die Synthese von Silylestern beschrieben. Das ferne IR einiger Ester wird angeführt; eine Untersuchung der Verschiebung der Carbonyl-Streck-Frequenz bei Kondensation zeigt keine signifikanten Unterschiede zwischen Methyl- und Silyl-Estern.相似文献
69.
The approaches to the synthesis of various 16,17-disubstituted pregna-4,9-dien-3,20-diones from the corresponding 9-derivatives with labile epoxide, dioxolane, and oxathiolane ringsD have been studied. The transformation has been found to proceed efficiently when the 9-sulfinic esters are used at the intermediate stage and then elimination of sulfinic acid by TsOH/SiO2 is carried out.For part 193, see ref. 7.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 983–986, May, 1993. 相似文献
70.
A modification of a procedure by Hage [1] is proposed for the gas chromatographic evaluation of the content of free medium-chain fatty acids and related ethyl esters in beer. The method involves extraction of free fatty acids and ethyl esters by SPE using C18 bonded phase columns, derivatization of free fatty acids and related ethyl esters with diazomethane, and GC analysis using an SP-2340 capillary column. The results obtained have shown the method to be rapid and highly reproducible. The technique has been compared with other methods used for determination of free fatty acids. 相似文献