Chiral separation of three agrochemical toxins enantiomers by high-performance liquid chromatography on a vancomycin crystalline degradation products-chiral stationary phase

This work aims to evaluate for the enantiomeric separations of three agrochemical toxins: haloxyfop-methyl, fenoxaprop-p-ethyl and indoxacarb on crystalline degradation products-chiral stationary phase (CDP-CSP) of high-performance liquid chromatography (HPLC) under normal and polar organic phases. In the normal phase, the mobile phase was n-hexane with alcohols including methanol and isopropanol as polar modifiers. In the polar organic phase mode, the mobile phase was methanol with different percentages of triethylammunium acetate. The influence of flow rate (0.3-0.9 mL/min), analyte concentration and silica gel particle sizes (10, 15 and 30 microm) was investigated. This new chiral stationary phase showed excellent stereoselectivity for the two enantiomers of haloxyfop-methyl and fenoxaprop-p-ethyl and chiral recognition for indoxacarb under normal-phase mode. However, under polar organic phase, only indoxacarb was separated (alpha < 1.5). The chromatographic results were compared with commercial chiral columns.     

Development of a Reversed-Phase Liquid Chromatographic Assay for the Quantification of Total Persipeptides in Fermentation Broth

The emergence and prevalence of multi-drug-resistant bacterial strains increase the potential for outbreaks of incurable infections. The discovery of novel antibiotics and pharmacological preparations requires the identification of novel bioactive small molecules. A specific, sensitive, and reliable quantification method using high-performance liquid chromatography (HPLC) with UV detection was developed for the determination of total persipeptides (A and B), which are cyclic pentapeptides found in the fermentation broth of Streptomyces zagrosensis UTMC 1154 that exhibit bioactivity against methicillin-resistant Staphylococcus aureus (MRSA). A simple liquid–liquid extraction (LLE) method using butanol was employed to extract persipeptides from the fermentation broth prior to HPLC analysis. The chromatographic separation of persipeptides and the internal standard, virginiamycin, was achieved with a gradient of acetonitrile and water on a C18 reversed-phase analytical column in a 25-min analytical run utilizing a flow rate of 0.8 mL min⁻¹ and detection at 210 nm. The whole assay was validated, and the method presented a linear response range with a regression coefficient of determination R ² of 0.9996 for the quantification of persipeptides in the concentration range of 3.9–250.0 µg mL⁻¹, as well as extraction recoveries ranging from 54.78 ± 9.83 % to 56.45 ± 16.33 %. The bias and the precision of the proposed method were <10 %. The detection and quantification limits for the persipeptides were 27 and 83 µg L⁻¹, respectively.

     

Preparation and characterization of new inorganic–organic hybrid catalyst H3PMo12O40/Hyd‐SBA‐15 and its application in the domino multi‐component reaction

We present novel inorganic–organic hybrid catalyst to accomplish domino multi‐component reaction (MCR) for synthesis of 3‐amino‐2′‐oxospiro[benzo[c]pyrano[3,2‐a]phenazine‐1,3′‐indoline]‐2‐carbonitrile/carboxylate derivatives. This methodology offers remarkable development by easy production of H₃PMo₁₂O₄₀/Hyd‐SBA‐15 in regard to solving the problem of using harsh catalysts, also it demonstrates to be impressive and environmentally friendly in term of low reaction times and high yields.     

Hydrodesulfurization unit for natural gas condensate

Journal of Thermal Analysis and Calorimetry - Nowadays, most of the world’s energy consumption is from fossil fuels. One of these fossil fuels is natural gas condensate which consists of...     

A novel one-pot synthesis of some new interesting pyrrole derivatives

[reaction: see text] 11-(1H-Pyrrol-1-yl)-11H-indeno[1,2-b]quinoxaline and 3-(1H-pyrrol-1-yl)indolin-2-one derivatives have been synthesized in good yields in a novel, one-pot, and efficient process by condensation of 11H-indeno[1,2-b]quinoxalin-11-one or isatin derivatives with 4-hydroxyproline on solid-support montmorillonite K10 under microwave irradiation.     

One‐pot three components synthesis of alkyl indeno [1,2‐b]‐quinoxalin‐11‐ylideneacetates in water and under solvent‐free conditions

We introduced a very simple, one‐pot three component procedure for preparation of alkyl indeno[1,2‐b]quinoxalin‐11‐ylideneacetates 4 from reaction of ninhydrin 1 , phenylenediamines 2 , (alkoxycarbonylmethyl)triphenylphosphonium bromides 3 , and sodium acetate in water and under solvent‐free conditions. © 2005 Wiley Periodicals, Inc. Heteroatom Chem 16:549–552, 2005; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20136     

Stripping voltammetry of thorium based on adsorptive accumulation

A sensitive stripping voltammetric procedure for quantifying thorium is described. The chelate of thorium with the azo dye Mordant Blue 9 is adsorbed on the hanging mercury drop electrode, and the reduction current of the accumulated chelate is measured during a negative-going potential scan. Cyclic voltammetry is used to characterize the interfacial and redox behaviors. The effects of pH, dye concentration and accumulation potential are discussed. The detection limit is 4 × 10^?10 M (4-min accumulation), a linear current-concentration relationship is observed up to 1.3 × 10^?7 M, and the relative standard deviation (at the 6 × 10^?8 M level) is 3.1%. Possible interferences by trace metals and organic surfactants are investigated. Simultaneous quantitation of thorium and nickel is illustrated.     

Improved Method for the Total Synthesis of Azaperone and Investigation of Its Electrochemical Behavior in Aqueous Solution

Azaperone, with anti-anxiety and anti-aggressive activities used in veterinary medicine, is a member of the butyrophenone class. It is ordinarily utilized for a wide range of indications, such as sedation, obstetrics, and anesthesia. In this research, an improved synthetic route is presented for azaperone using a phase-transfer catalyst(PTC). In general, it was synthesized as a dopamine antagonist in four steps. The bis(2-chloroethyl) amine intermediate is easily obtained after the conversion of the alcohol groups into the chloride leaving group using thionyl chloride(95% yields). The alkylation of commercially available 2-amino pyridine in the presence of PTC was then carried out, giving 1-(pyridin-2-yl) piperazine with 75% yield. 1-(Pyridin-2-yl) piperazine was finally alkylated using 4-chloro-1-(4-fluorophenyl) butan-1-one to achieve azaperone with 60% yield. The butyrophenone intermediate was obtained via the Friedel-Crafts reaction of fluorobenzene with 4-chlorobutyryl chloride in the presence of AlCl₃. High efficiency, gentle reaction conditions, and fast and simple procedure are the advantages of this method. Also, the electrochemical oxidation behaviour of azaperone was investigated using cyclic and differential pulse voltammetry techniques. Cyclic voltammetric studies indicated an irreversible process for azaperone electro-oxidation with a peak potential of 0.78 V in a phosphate buffer solution(pH=7.0) vs. Ag/AgCl(saturated KCl) electrode. The value of the peak current vs. the azaperone concentration was enhanced linearly in the range of 10―70 μmol/L, and the detection limit was found to be 3.33 μmol/L.     

Modified Eu3+ doped Y2O3 Nanoparticles as Turn-on Fluorescence Sensor for Sensitive Determination of Methamphetamine

Journal of Analytical Chemistry - In this article, a new spectrofluorometric method was developed for the determination of methamphetamine based on a turn-on luminescence response of captopril...     

Automated hollow‐fiber liquid‐phase microextraction followed by liquid chromatography with mass spectrometry for the determination of benzodiazepine drugs in biological samples

In this study, two‐phase hollow‐fiber liquid‐phase microextraction and three‐phase hollow‐fiber liquid‐phase microextraction based on two immiscible organic solvents were compared for extraction of oxazepam and Lorazepam. Separations were performed on a liquid chromatography with mass spectrometry instrument. Under optimal conditions, three‐phase hollow‐fiber liquid‐phase microextraction based on two immiscible organic solvents has a better extraction efficiency. In a urine sample, for three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents, the calibration curves were found to be linear in the range of 0.6–200 and 0.9–200 μg L^?1 and the limits of detection were 0.2 and 0.3 μg L^?1 for oxazepam and lorazepam, respectively. For two‐phase hollow fiber liquid‐phase microextraction, the calibration curves were found to be linear in the range of 1–200 and 1.5–200 μg L^?1 and the limits of detection were 0.3 and 0.5 μg L^?1 for oxazepam and lorazepam, respectively. In a urine sample, for three‐phase hollow‐fiber‐based liquid‐phase microextraction based on two immiscible organic solvents, relative standard deviations in the range of 4.2–4.5% and preconcentration factors in the range of 70–180 were obtained for oxazepam and lorazepam, respectively. Also for the two‐phase hollow‐fiber liquid‐phase microextraction, preconcentration factors in the range of 101–257 were obtained for oxazepam and lorazepam, respectively.