A study of the viability of three derivatizing reagents for obtaining amino acid profiles in honey through high performance liquid chromatography (HPLC) is presented. A method using diode array detection based on a reaction with diethyl ethoxymethylene malonate (DEMM) and two other methods using fluorescence detection based on derivatization with fluorenylmethyl chloroformate (FMOC-Cl) and 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) have been developed. The three methods yield detection limits close to the ppb level, but vary in relation to other analytical characteristics. The use of methyl chloroformate derivatives allows the profile to be obtained with the greatest sensitivity within a short time frame. On applying such methods to honey samples of diverse botanical origin, we observe that the proline values obtained are always lower than those found using the official spectrophotometric method, thereby underlining the advisability of using HPLC methods to reduce uncertainty in these results. 相似文献
A rapid access to carbocyclic nucleosides containing a fused isoxazoline ring is proposed starting from cyclopentadiene. The route involves an hetero Diels-Alder cycloaddition reaction of nitrosocarbonylbenzene followed by a 1,3-dipolar cycloaddition of nitrile oxides, cleavage of the N-O tether and elaboration of the heterocyclic aminols into nucleosides via linear construction of purine and pyrimidine heterocycles. 相似文献
Organomercury fulminates react with acetylene derivatives to give unstable 3-(organomercurio)isoxazoles, which isomerize to 2-cyanoenolates. These are hydrolyzed with hydrochloric acid to the corresponding enols and are cleaved by water at the double bond. With monosubstituted acetylenes, substitution at the free position by the organomercury residue is predominant. 相似文献
An automated flow injection analysis (FIA) system for quantifying ethanol was developed using alcohol oxidase, horseradish
peroxidase, 4-aminophenazone, and phenol. A colorimetric detection method was developed using two different methods of analysis,
with free and immobilized enzymes. The system with free enzymes permitted analysis of standard ethanol solution in a range
of 0.05–1.0 g of ethanol/L without external dilution, a sampling frequency of 15 analyses/h, and relative SD of 3.5%. A new
system was designed consisting of a microreactor with a 0.91-mL internal volume filled with alcohol oxidase immobilized on
glass beads and an addition of free peroxidase, adapted in an FIA line, for continued reuse. This integrated biosensor-FIA
system is being used for quality control of biofuels, gasohol, and hydrated ethanol. The FIA system integrated with the microreactor
showed a calibration curve in the range of 0.05–1.5 g of ethanol/L, and good results were obtained compared with the ethanol
content measured by high-performance liquid chromatography and gas chromatography standard methods. 相似文献
Conductance measurements are reported for LiPi, NaPi, KPi, RbPi, CsPi, Bu4NPi, Bu4NBr, Bu4NClO4, Bu4NNO3, and Bu4NBBu4 at 25°C in -butyrolactone-sulfolane mixtures. In these mixtures of solvents that are practically homomorphous, isodielectic and with comparable dipole moments, the ion pair association and ionic mobilities of large ions conform to the expectations of the primitive model. Electrolytes containing lithium or sodium ions show anomalies indicating that other factors besides shape, dipole moment, and polarizability of the solvent molecules are involved in the association and transport processes of these ions. 相似文献
Summary The synthesis and the dinuclear or mononuclear nature of several molybdenum(VI) and molybdenum(V) oxocomplexes derived from 1,3-diphenyl-1,3-propanedione (HLL) are described. These complexes were identified by i.r. and electronic spectra, magnetic susceptibility and analytical data, and are assigned the following formulae: [MoO2(LL)2], [Mo2O5(LL)2], [Mo2O4(LL)2], [MoOCl(LL)2], [MoCl2(LL)] and [MoO(OH)(LL)2)]. The low magnetic moments of the dinuclear complexes are due, in part, to intramolecular interactions. The i.r. data show that the dionate is bound by two oxygen atoms forming a chelate six-membered ring. 相似文献
EtO? in DMSO adds to ethylthiopicrate at C-3 to generate an ephemeral -adduct which ends into 1-ethylthio-4-ethoxy-2,5-dinitrobenzene, whilst ethyl picrate gives two adducts of attack of EtS? at C-3 or C-1. 相似文献