Development of GC–MS/MS method with programmable temperature vaporization large volume injection for monitoring of 17β-estradiol and 2-methoxyestradiol in plasma

Monitoring of estradiol and its metabolites in biological samples is essential for the accurate diagnosis of a number of endocrine diseases. In this study, a sensitive, precise and specific GC–MS/MS method for the quantification of 17β-estradiol (17-BE) and its main metabolite, 2-methoxyestradiol (2-MEOE), in plasma was developed and validated. Plasma concentrations of these steroids are currently investigated as diagnostic markers for pre-eclampsia, a systematic disorder of pregnancy and a leading cause of maternal and fetal morbidity and mortality worldwide.     

Use of a Tensammetric Wave for the End-Point Detection in Chelatometry

Abstract

A new method for the end-point detection in complexometric titration using a tensammetric wave of organic reagents such as oxine and alizarin complexone (ALC) was studied. The tensammetric wave of these reagents disappears by their chelate formation and reappears by the liberation of free indicator during the exchange reaction between indicator chelate and EDTA. This mechanism is utilized for the end-point detection in complexometric titration of metals. Since the sensitivity of tensammetric wave is extremely high, very sharp end-point can be obtained for the titration of metals even in the concentration of 10^?5M.     

TiO2/activated carbon fibers photocatalyst: Effects of coating procedures on the microstructure, adhesion property, and photocatalytic ability

In order to more easily separate TiO₂ photocatalyst from the treated wastewater, TiO₂ film was immobilized on the surface of activated carbon fibers (ACFs) by employing two kinds of coating procedures, dip-coating, and hydrothermal treatment. The effects of coating procedures on microstructure of TiO₂-coated ACFs (TiO₂/ACFs), such as morphology, porous property, crystal structure, and light absorption characteristics were investigated in detail. The adhesion property between TiO₂ film and ACFs was evaluated by ultrasonic vibration, and the photocatalytic activity of TiO₂/ACFs was tested by the photocatalytic decoloration of methylene blue solution. The results show that hydrothermal treatment presented many advantages to obtain high-performance TiO₂/ACFs photocatalyst in comparison with dip-coating. Hydrothermal treatment could improve the binding property between TiO₂ films and ACFs, which endowed the as-obtained TiO₂/ACFs photocatalyst with improved reusable performance, and TiO₂/ACFs synthesized by hydrothermal treatment presented higher photocatalytic activity.     

Zinc-catalyzed benzylic C-H bond oxidation

A zinc-catalyzed oxidation of benzylic substrates has been developed. The corresponding carbonyl containing compounds have been produced in moderate to excellent yields. Both arenes and heteroarenes can be applied as substrates by using H₂O₂ as the oxidant.     

Fluorimetric Analysis of Aluminum in Diluted Hemodialysis Solutions by Using a Novel Schiff Base

A spectrofluorimetric method has been developed for trace amount of aluminum(III) by using a novel Schiff base, N,N′-bis(salicylidene)-1,4-diaminobuthane (BUTAS), and 4-methyl-2-aminophenol (OAP). Since the aluminum complexes are generally fluorescent, aluminum(III) increases the fluorescence intensity of BUTAS-OAP by formation of Al-BUTAS-OAP complex. The fluorescence of the complex is measured at an excitation wavelength of 410 nm with an emission at 526 nm. Aluminum(III) can be detected within a concentration limit of 0.11–1.62 ppb and the lowest detection limit being 0.07 ppb. The proposed method was applied to diluted hemodialysis solution and spectrofluorimetric data was compared with data of standard pharmacopoeia method.     

Syntheses and molecular structures of four inorganic–organic hybrid compounds from N-containing aromatic bases and perchlorometallates of Zn,Cu, Sn,and Fe

Four organic–inorganic crystals, [(HL1)₂(ZnCl₄)]·H₂O (1) (L1?=?2-methylquinoline), [(HL1)₂(CuCl₄)] (2), [(HL2)₂SnCl₆] (3) (L2?=?6-bromobenzo[d]thiazol-2-amine), and [(HL3)FeCl₄] (4) (L3?=?5,7-dimethyl-1,8-naphthyridine-2-amine), derived from N-containing aromatic Brønsted bases and metal(II) chlorides (zinc(II) chloride, copper(II) chloride dihydrate, tin(II) chloride dihydrate, and iron(III) chloride hexahydrate) were prepared at room temperature and characterized by IR, X-ray structure analysis, elemental analysis, and TG analysis. The crystals are built up by perchlorometallates (Zn, Cu, Sn, and Fe) associated with organic cations through multiple non-covalent associations. X-ray diffraction analysis reveals that 1 and 2 have 3-D network structures built from hydrogen bonds between the cations and chlorometallates. Water molecules play an important role in structure extension in 1. Anhydrous 3 and 4 produced from 2-aminoheterocyclic derivatives display 2-D sheet structures. Arrangements of anions and cations are dominated by shape and size of cations, and also by the different structures of the chlorometallates as well as non-bonding interactions in the crystal structures. Except for 1, the other compounds are thermally stable below 240°C.     

A Sensitive Spectrophotometric Method for the Determination of Some Imidazoline Derivatives by 2,6-Dichlorophenol-Indophenol

Abstract

A new and highly sensitive method is presented for the spectrophotometric determination of four imidazoline derivatives: antazoline hydrochloride, tolazoline hydrochloride, xylometazoline hydrochloride and naphazoline nitrate. The method is based on the reaction of the corresponding drug base with 2,6 - dichlorophenol -indophenol (DGPIP) in chloroform to give a blue chromogen exhibiting a maximum at 588 - 603nm. The method could be applied for the quantitative determination of the above drugs either pure or in their pharmaceutical preparations (tablets and nasal drops). The results obtained are accurate and have good reproducibility.     

Statistical methods for improving verification of claims of origin for Italian wines based on stable isotope ratios

Wine derives its economic value to a large extent from geographical origin, which has a significant impact on the quality of the wine. According to the food legislation, wines can be without geographical origin (table wine) and wines with origin. Wines with origin must have characteristics which are essential due to its region of production and must be produced, processed and prepared, exclusively within that region.     

Two new β-carboline-type alkaloids from Stellaria dichotoma var.lanceolata

Two new β-carboline-type alkaloids,dichotomine K(1) and dichotomine L(2),were isolated from the roots of Chinese medicinal plant Stellaria dichotoma L.var.lanceolata Bge.Structures of 1 and 2 were determined on the basis of chemical and spectroscopic means.     

Novel and efficient supramolecular synthesis of pyrroles in the presence of β-cyclodextrin in water

A simple and efficient synthesis of highly substituted pyrroles was achieved in water medium via multi-component strategy, using amine,DMAD/DEAD as well as phenacyl bromide catalyzed by β-CD.Utilizing this protocol various pyrrole derivatives were synthesized in good to excellent yields.