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71.
T P Davis C W Gehrke C W Gehrke T D Cunningham K C Kuo K O Gerhardt H D Johnson C H Williams 《Journal of chromatography. A》1979,162(3):293-310
A remarkably sensitive, simple and selective reversed-phase high-performance liquid chromatographic (HPLC) method has been developed, allowing, for the first time, the direct measurement of histamine, norepinephrine, octopamine, normetanephrine, dopamine, serotonin and tyramine in a single sample of plasma (2 ml), tissue (0.2 g), or urine. The biogenic amines were modified by pre-column derivatization with o-phthalaldehyde which stabilizes the molecules, aids in extraction, and improves HPLC detection at the nanogram level. To minimize losses during the sampling procedure a careful collection procedure was designed. We developed a simple sample cleanup in which the samples were thawed, neutralized with KOH, immediately derivatized, extracted into ethyl acetate (EtOAc) and then chromatographed by HPLC. The derivatives were stable in EtOAc for more then 24 h. Interfering amino acids were removed from the EtOAc by partitioning twice with Na2HPO4 buffer (pH 10.0). Complete separation was achieved in ca. 60--90 min on a muBondapak phenyl column using a stepwise gradient of acetonitrile and/or methanol-phosphate buffer (pH 5.1). A variable wavelength fluorometer with a 5-microliter flow-cell was used (excitation 340 nm; emission 480 nm). Linearity ranged from 200 pg to 50 ng onto the column. Precision (R.S.D.) for retention times was 1% and for derivatization and injection 2.5%. Recoveries of the seven biogenic amines from plasma spiked with 25 ng/ml averaged 70%, with a relative standard deviation of 6%. Separation studies were also done using a muBondapak C18 column. The effects of various eluents are presented. Gas-liquid chromatography was also investigated but lacked the sensitivity achieved by HPLC. The HPLC method is used routinely for the determination of biogenic amines in plasma from pigs with malignant hyperthemia and thermally stressed bovine. Significant differences in levels of biogenic amines were noted between stressed and non-stressed animals. Data on rat brain tissue samples were compared with the trihydroxyindole method and canine heart tissue was analyzed for ventricular norepinephrine and dopamine. Application of the method to urine from normal persons and a patient with a brain tumor has been demonstrated. 相似文献
72.
Monoanionic tridentate ligands LHa and LHb containing ONSe and ONTe donor sequences and their Pd2+ and Pt2+ derivatives were synthesized and characterized. The formation of a five- and a six-membered ring around the central metal atom and associative phenomena in solutions provide extra stability to the metal complexes. 相似文献
73.
Miss Itawati Pratanata L. R. Williams R. N. Williams 《Journal of mass spectrometry : JMS》1974,9(4):418-421
When subjected to electron-impact, chloromethyl aryl sulphones (II, X = Cl) fragment predominantly by the loss of CH2Cl from the molecular ion followed by the loss of SO2 and in most cases the appropriate metastable peaks are present to confirm the transitions. In addition, alkyl–oxygen bond formation in the molecular ion was revealed by the presence of prominent peaks corresponding to the [R? ?-SO]+ ions. In most spectra no evidence for aryl–oxygen bond formation could be found and thus the presence of the chlorine atom was able to effectively reverse the direction of skeletal rearrangement reported for aryl methyl sulphones. 相似文献
74.
[formula: see text] The diastereoselective synthesis of cis-2,5-disubstituted-3-methylenetetrahydrofurans via Pd(0)-catalyzed cyclization of 2-methylene-1,4-diols is described. Investigations into the scope of the reaction and its application toward the synthesis of amphidinolide K is reported. 相似文献
75.
1,1-Diaryl-1-penten-4-yn-3-ols react with diphenylphosphine oxide in the presence of a thiolate-bridged diruthenium complex as a catalyst and give high yields of aryl(diphenyl)phosphine oxide products via an initial substitution followed by a cyclization at the produced allene intermediate. [reaction: see text] 相似文献
76.
The ADE fragment of nakadomarin A has been synthesized in nine linear steps from commercial material. The key transformation is an asymmetric azomethine ylide [1,3]-dipolar cycloaddition to establish the AD-spirocyclic system containing three of the four stereocenters of the natural product. [reaction: see text] 相似文献
77.
[reaction: see text] Double phosphinylation of propargylic alcohols with diphenylphosphine oxide in the presence of a thiolate-bridged diruthenium complex as catalyst gives the corresponding 2,3-bis(diphenylphosphinyl)-1-propenes in high yields with a complete selectivity. 相似文献
78.
The arylation of fluorobenzene with pentafluorophenyl radicals obtained by the reaction of the corresponding aniline with pentyl nitrite is described. The reaction involves attact at the 2t?-,3t?-and 4t?-positions. The composition of the mixture and the nature of its components were determined by 19F NMR spectroscopy and were confirmed by gas-liquid chromatography. 相似文献
79.
Dudley Williams and his colleagues discuss how ligands can gain binding energy to their receptors, and substrate transition states to their enzymes, by tightening the protein structures, with a decrease in their dynamic behaviour. 相似文献
80.
Eva Eichler Clarence Stanley Rooney Haydn Windsor Richard Williams 《Journal of heterocyclic chemistry》1976,13(4):841-844
The syntheses of some 1,8-naphthyridines substituted in the 6-position with heterocyclic groups are described. A synthetic route to 6-amino-5,7-dimethyl-1,8-naphthyridin-2(1H)one is also presented. 相似文献