MASS SPECTROMETRIC STUDIES ON SPIROCYCLIC DERIVATIVES OF CYCLODIPHOSPH(V)AZANES

Abstract

The formation and subsequent fragmentation of spirocyclodiphosph(V)azanes (II-III) has been studied by mass spectrometry using the link-field scan technique and structural inferencies are drawn from these data. ³¹P nmr measurements for compound (III) are also described.     

Dynorphin A 1–17 biotransformation in inflamed tissue, serum and trypsin solution analysed by liquid chromatography–tandem mass spectrometry

Dynorphin A 1–17 (DYN A) is an endogenous neuropeptide that is of interest due to its diverse roles in analgesia, inflammation and addiction. Upon release, DYN A is subject to metabolism by a range of enzymes and its biotransformation is dependent on the site and environment into which it is released. In this study, we investigated the biotransformation of DYN A in rat inflamed tissue at pH?7.4 and 5.5, in rat serum and in trypsin solution. DYN A-porcine was incubated at 37?°C in each matrix over a range of incubation periods. The resultant fragments were separated using a C4 column and detected by mass spectrometry using total ion current mode. Incubation of DYN A in trypsin solution and in rat serum resulted in 6 and 14 fragments, respectively. Incubation in inflamed rat paw tissue occasioned 21 fragments at pH?7.4 and 31 fragments at pH?5.5. Secondary breakdown of some larger primary fragments was also observed in this study.     

FTIR analysis of the hydrolysis rate in the sol–gel formation of gadolinia-doped ceria with acetylacetonate precursors

This study reveals that Fourier transform infrared is an effective analytical tool in probing the extent of hydrolysis of cerium and gadolinium acetylacetonates dissolved in methanol. It is found that these acetylacetonates have relatively fast hydrolysis rates at the early stage of hydrolysis (<6 h). However, their hydrolysis rates become very slow beyond 6-h of hydrolysis and decrease to near zero after 55-h of hydrolysis. As a result, hydrolysis cannot be completed even after 170 h at room temperature. These phenomena suggest that the first and second acetylacetone ligands chelated to Ce³⁺ and Gd³⁺ ions can actually be hydrolyzed with relative ease at room temperature, similar to alkoxide ligands. It is the last acetylacetone ligand that is very difficult to be hydrolyzed.     

AN INVESTIGATION OF THE REACTION PRODUCTS OF N3P3CL4(NH2)2 WITH NUCLEOPHILIC REAGENTS. EXAMPLES OF GEMINAL → NON-GEMINAL REARRANGEMENTS

Abstract

Based on its reactions with various nucleophiles both geminal and non-geminal structures have been earlier proposed for N₃P₃Cl₄(NH₂)₂, although its geminal structure is now considered established. The reactions of this compound with alcohols have been investigated and the products examined by NMR spectroscopy and X-ray crystallography. Evidence for both unrearranged as well as geminal → non-geminal rearranged alcoholysis products is presented.     

PHOSPHORUS-NITROGEN COMPOUNDS. PART 52.1 THE SYNTHESIS OF SOME 1,3,2-BENZODIAZAPHOSPHORINE 2-OXIDES AND 2-SULPHIDES

Abstract

The reactions of 4-methyl-2-[N-(p-toluidinyl)methyl]aniline with phosphorus oxychloride, thiophosphoryl chloride, and their derivatives yield 1,3,2-benzodiazaphosphorine 2-oxides and 2-sulphides. Their ¹H NMR and infrared spectra are discussed. Related 1,3,2-benzodiazophosphorine and 1,3,2-dibenzodiazaphosphocine 2-oxides and 2-sulphides are compared.     

Biochemical and Structural Studies of Conserved Maf Proteins Revealed Nucleotide Pyrophosphatases with a Preference for Modified Nucleotides

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A bis(rhodamine 6G)-based fluorescent sensor for Hg2+: microwave-assisted synthesis,photophysical properties,and computational studies

A fluorescent and colorimetric sensor based on rhodamine 6 g (RD6g) was designed, synthesized, and characterized using microwave irradiation. The sensing behavior of this compound was studied by UV–visible and fluorescence spectroscopy. Sensor RD6g exhibits a high selectivity and an excellent sensitivity and is a dual-responsive colorimetric and fluorescent Hg²⁺-specific sensor in aqueous buffer solution. Mercury ions give rise to the development of a very fluorescent ring-open amide spirolactam system. The detection limit for Hg²⁺ was found to be 1.2?×?10^?8 M. The binding ratio of RD6g-Hg²⁺ complex was determined to be 1:1 according to the Job’s plot. The reversibility of RD6g?Hg²⁺ complex has been achieved with CN^? anions. The test strip based on RD6g was developed, which could be used as a suitable and methodical Hg²⁺ test kit.