Determination of theophylline and its metabolites in biological samples by liquid chromatography-mass spectrometry

Liquid chromatography–mass spectrometry (LC–MS) is a powerful tool for analysis of drugs and their metabolites. We used a column-switching system in combination with atmospheric pressure chemical ionization LC–MS (LC–APCI–MS) for the determination of theophylline and its metabolites in biological samples. The separation was carried out on a reversed-phase column using methanol–20 mM ammonium acetate as a mobile phase at a flow-rate of 1 ml/min in 30 min. In the mass spectrum, the molecular ions of these drugs and metabolites were clearly observed as base peaks. This method is sufficiently sensitive and accurate for the pharmacokinetic studies of these drugs.     

Inequalities for a distribution with monotone hazard rate

Summary LetX be a positive random variable with the survival function and the densityf. LetX have the moments μ=E(X) and μ₂=E(X ²) and put ε=|1-μ₂/2μ²|. Put and . It is proved that the following inequalities hold: , for allx>0, ifq(x) is monotone and that , ifq ₁ (x) is monotone. It is also shown that Brown's inequality which holds wheneverq ₁ (x) is increasing is not valid in general whenq ₁ is decreasing. The Institute of Statistical Mathematics     

Selective syntheses of metalated pyridines from two different unsymmetrical acetylenes, a nitrile, and a titanium(II) alkoxide

Cyclotrimerization of two different, unsymmetrical acetylenes and p-toluenesulfonylnitrile with a divalent titanium alkoxide reagent, Ti(O-i-Pr)4/2 i-PrMgCl, yielded single pyridyltitanium compounds in a highly selective manner. These metalated pyridines were confirmed by deuteriolysis to give the corresponding deuterated pyridines and underwent iodinolysis and copper-catalyzed alkylation to demonstrate their synthetic utility. Alternatively, a different type of cyclotrimerization of an alkynamide, terminal acetylenes, and alpha-alkoxynitriles mediated by the same titanium(II) alkoxide again proceeded in a highly selective manner to give single pyridines having a titanated side chain.     

The autorecycling oxidation of benzylamine by synthetic 8-hydroxy-5-deazaflavin derivatives

Various 8-hydroxy-5-deazaflavin derivatives were synthesized as the model compounds of coenzyme F₄₂₀-These compounds oxidized benzylamine to benzaldehyde more efficiently than the corresponding 8-unsubstituted 5-deazaflavins.     

Thermomechanical analysis of a polymer dispersed liquid crystal containing a thermoplastic elastomer

Bulk samples of polymer dispersed liquid crystals (PDLCs) containing polystyrene (PS) and a thermoelastic elastomer as polymer matrices, have been prepared by a thermally-induced phase separation method. Thermomechanical analysis measurements revealed that the PDLC containing the thermoplastic elastomer possessed rubber-like elasticity even in the mesomorphic temperature range of the LC while the PDLC based on PS showed plastic deformation during the measurement.     

The effect of bath pH on electrodeposition and corrosion properties of ternary Fe-W-Zn alloy platings

Journal of Solid State Electrochemistry - As a new trial to improve the corrosion resistance of the Fe-W alloy platings, Fe-W alloys incorporating a small amount of Zn, namely novel ternary Fe-W-Zn...     

Measurement of the change in partial molar volume during electrode reaction by gravity electrode—II. Examination of the accuracy of the measurement

The reliability of the measurement of the change in partial molar volume between product and reactant ions measured by gravity electrode (GE) was examined by the thermodynamic measurement of pycnometer (PM). Since the PM method requires an experimental equation of the apparent molar volume to calculate the partial molar volumes of the individual ions, the most suitable experimental equation must be first determined. As a test reaction for the experiment, oxidation of ferrocyanide (FERO) ion to ferricyanide (FERI) ion was adopted. After fitting several experimental equations to the data of the apparent molar volumes by the PM method, the calculated changes in the partial molar volume were compared with the data of the GM method. Then, it is concluded that the polynomial with a degree of 3 of the logarithm of the molality of the FERO ion suggests the most suitable equation. As a result, the reliability of the GE method was also experimentally validated.     

Intense fluorescence-inducing amphiphile in cationic dyes and its applicability

An anionic amphiphile has been found to form extremely hydrophobic sites in water and specifically incorporate stilbazolium-based compact hemicyanine dyes as monomeric species, resulting in induction of intense fluorescence emission.     

Studies on nepalese crude drugs. XXVIII. Chemical constituents of Bhote Khair, the underground parts of Eskemukerjea megacarpum HARA

From the underground parts of Eskemukerjea megacarpum HARA, two new stilbenes (14, 15) were isolated, together with a known coumarin, 5,7-dihydroxycoumarin (1), a tyramine derivative, trans-feruloyltyramine (2), two pyrogallol derivatives, gallic acid (3) and beta-glucogallin (4), four flavonoids, trifolin (5), hyperin (6), myricetin 3-O-beta-D-galactopyranoside (7), and myricitrin (8), five stilbenes, resveratorol (9), astringenin (10), piceid (11) astringin (12), and resveratorol 3-O-beta-D-(6-O-galloyl)glucopyranoside (13), a flavan-3-ol, (-)-epigallocatechin 3-O-gallate (16), two proanthocyanidins, catechin-(4alpha-->8)-epigallocatechin 3-O-gallate (17) and epicatechin 3-O-gallate-(4beta-->8)-epigallocatechin 3-O-gallate (18), and an anthocyanin, idaein (19). Compounds 14 and 15 were identified as (E)-3,5,3',4'-tetrahydroxystilbene 3-O-beta-D-(6-O-galloyl)glucopyranoside and (E)-3,5,4'-trihydroxystilbene 3-O-beta-D-(6-O-galloyl)glucopyranoside, respectively, based on spectral and chemical data.