Determination of Folic Acid by CE in Various Cultivated Variety of Lentils

A simple extraction and determination method for folic acid (FA) in lentil samples was developed employing capillary electrophoresis. The analysis was performed in a 75 μm ID fused silica capillary using a running buffer of 10 mM sodium borate (10%, v/v, methanol, pH 9) at +18 kV and a detection wavelength at 200 nm. Methylparaben was used as the internal standard. FA signal response was linear in the range between 1.2 × 10^?5 and 4.8 × 10^?5 M. Limit of detection (inter-day) was determined at 6.12 × 10^?7 M (3.3 σs^?1). The amount of FA found in green, red and mignon lentils was found to range between 0.408 and 0.742 mg g^?1.     

Adsorption of isoniazid onto sepiolite–palygorskite group of clays: An IR study

The adsorption of isoniazid (INH) on sepiolite, loughlinite (natural Na-sepiolite) and palygorskite from Anatolia was investigated by FT-IR spectroscopy. Experimental results indicated that INH molecules, adsorbed on sepiolite–palygorskite group of clays, are coordinated to surface hydroxyls by H-bonding interaction through the pyridine ring nitrogen lone pairs. Moreover, some of the adsorbed INH molecules may enter the interior channels of the sepiolite–palygorskite structure and involve H-bonding interaction with zeolitic water. Some intensity and frequency changes in the OH stretching band of surface hydroxyls (Si–OH) of the INH-treated sepiolite and loughlinite were observed. However, this band is found to be less affected by the adsorption of isoniazid in the case of palygorskite, probably because the surface Si–OH groups in palygorskite appear to be less abundant than in sepiolite or loughlinite.     

Preconcentration of uranium(VI) and thorium(IV) from aqueous solutions using low-cost abundantly available sorbent

Olive cake as low-cost abundantly available sorbent has been characterized by N₂ at 77 K adsorption, porosity analysis, elemental analysis and IR spectra and has been used for preconcentrating of uranium(VI) and thorium(IV) ions prior to their determination spectrophotometrically. The optimum pH values for quantitative sorption of U(VI) and Th(IV) are 4–7 and 3–7, respectively. The enrichment factor for the preconcentration of U(VI) and Th(IV) were found to be 125 and 75 in the given order. The sorption capacity of olive cake is in the range of 2,260–15,000 μg g⁻¹ for Th(IV) and in the range of 1,090–17,000 μg g⁻¹ for U(VI) at pH 3–7. The sorbent exhibits good reusability and the uptake and stripping of the studied ions were fairly rapid. The elution of U(VI) and Th(IV) was performed with 0.3–1 M HCl/1–2 M HNO₃ and 0.3–0.8 M HCl/1 M HNO₃, respectively. The precision of the method was 1.8 RSD% for U(VI) and 2.5 RSD% for Th(IV) in a concentration of 1.00 μg mL⁻¹ for 10 replicate analysis. The influence of some electrolytes and cations as interferents was discussed. Separation of U(VI) and Th(IV) from other metal ions in synthetic solution was achieved.     

Lead Fractionation Analysis in Lipstick Samples by Inductively Coupled Plasma-Mass Spectrometry

A new analytical approach based on fractionation was introduced for lead in lipstick samples. Different separation techniques including n-hexane, glycerol extraction, and activated carbon adsorption were used to characterize the lipid fraction, polar and aromatic components of the samples. Additionally, artificial saliva and food stimulant extractions were used for the risk assessment studies. Trace metal levels in fractions were determined by inductively coupled plasma-mass spectrometry. Method validation parameters in the total element determinations were defined in terms of detection limits, accuracy, and precision. The limits of detection and quantification were 0.02 and 0.07 mg kg^?1 for Pb; whereas the repeatability and reproducibility of the results based on percent relative standard deviation were 3.0% and 7.2% for lead, respectively.     

Effect of conjugated core building block dibenzo[a,c]phenazine unit on π‐conjugated electrochromic polymers: Red‐shifted absorption

A comparative investigation was undertaken for the electrosynthesis and electrochemical properties of three different electroactive polymers having a conjugated core building block, dibenzo[a,c]phenazine. A series of monomers has been synthesized as regards to thiophene based units; thiophene, 3‐hexyl thiophene, and 3,4‐ethylenedioxythiophene. The effects of different donor substituents on the polymers' electrochemical properties were examined by cyclic voltammetry. Introducing highly electron‐donating (ethylene dioxy) group to the monomer enables solubility while also lowering the oxidation potential. The planarity of the monomer unit enhances π‐stacking and consequently lowering the E_g from 2.4 eV (PHTP) to 1.7 (PTBP). Cyclic voltammetry and spectroelectrochemical measurements revealed that 2,7‐bis(4‐hexylthiophen‐2‐yl)dibenzo[a,c]phenazine (HTP) and 2,7‐bis(2,3‐dihydrothieno[3,4‐b][1,4]dioxin‐5‐yl)dibenzo[a,c]phenazine (TBP) possessed electrochromic behavior. The colorimetry analysis revealed that while PTBP have a color change from red to blue, PHTP has yellow color at neutral state and blue color at oxidized state. Hence the presence of the phenazine derivative as the acceptor unit causes a red shift in the polymers' absorption to have a blue color. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 1714–1720, 2010     

Poly(HEMA-co-AA) microparticles for removal of aluminum: The reason for Alzheimer's

Aluminum is one of the most toxic metals causing a variety of neurologic diseases, especially Alzheimer's disease. It is impossible to avoid contact with aluminum because of its existence in food to medications. Therefore, removal of aluminum from the blood or wastewater is urgently important. The cost-effective and easy-to-prepare adsorbents are needed to get efficient aluminum removal. For that purpose, the poly(2-hydroxyethylmethacrylate-co-acrylic acid), poly(HEMA-co-AA), microparticles was synthesized to remove aluminum in a very short interaction time. The achievement of the desired polymeric structure was confirmed via Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and transmission electron microscope (TEM), etc. Additionally, particle features such as swelling ratio, size, and surface area were determined. The microparticles synthesized in this study have been determined with very good adsorption capacity even in small aluminum concentrations.     

Synthesis of new donor-acceptor polymers containing thiadiazoloquinoxaline and pyrazinoquinoxaline moieties: low-band gap, high optical contrast, and almost black colored materials

Two low band gap conjugated polymers, poly[4,9-bis(4-hexylthien-2-yl)-6,7-di(thien-2-yl)-[1,2,5]thiadiazolo[3,4-g]quinoxaline] (PHTTQ) and poly[5,10-bis(4-hexylthien-2-yl)-2,3,7,8-tetra(thien-2-yl)pyrazino[2,3-g]quinoxaline] (PHTPQ), consisting of alternating electron-rich 3-hexylthiophene and electron-deficient 6,7-di(thien-2-yl)-[1,2,5]thiadiazolo[3,4-g]quinoxaline (TTQ) and 2,3,7,8-tetra(thien-2-yl)-2,3-dihydropyrazino[2,3-g]quinoxaline (TPQ) units were synthesized electrochemically. The structures of the π-conjugated monomers were tailored using thiophene as the pendant group on the acceptor units (TTQ and TPQ). The electrochemical and optical properties of the polymers were investigated by cyclic voltammetry and UV-vis-NIR spectroscopy. The absorption spectra of PHTPQ, revealing a 1.0 eV band gap, exhibited three maxima at 352 nm, 535 nm, and 750 nm. Consequently, its absorption spectra cover the region between 400 and 800 nm, which make the polymer almost black in appearance. PHTTQ shows a λ_max value of 820 nm and a band gap of 0.8 eV which is very low among other [1,2,5]thiadiazolo[3,4-g]quinoxaline-containing donor-acceptor type polymers.     

Determination of some phthalate acid esters in artificial saliva by gas chromatography-mass spectrometry after activated carbon enrichment

The determination of six phthalate acid esters was achieved in artificial saliva using gas chromatography-mass spectrometry following activated carbon enrichment of samples. Central composite experimental design was applied to optimize method parameters, such as pH, adsorption time and amount of activated carbon. The best compromise of analytical conditions for the simultaneous determination of analytes from spiked artificial saliva were found to be: pH (3), adsorption time (30 min), activated carbon amount (1.8 g L⁻¹) and elution solvent (chloroform). These conditions were applied to study the migration of phthalate acid esters from different children's toys into saliva. A horizontal agitation method was applied to extract the analytes from plastic toys into saliva for 2 h at 37 °C. The detection limits of the method were in the range of 1.3-5.1 μg L⁻¹, while the relative standard deviation (%) values for the analysis of 100 μg L⁻¹ of the analytes were below 3.0% (n = 5). Di-2-ethylhexyl phthalate was the main analyte found in these samples.     

Structural properties of new spiro-1,3-propanediaminocyclotriphosphazene derivatives

New 1,3-propanediaminocyclotriphosphazene derivatives (7-17) were synthesized from the reactions of spiro-1,3-propanediaminocyclotriphosphazene, N₃P₃Cl₄[NH(CH₂)₃NH] (1) with the cyclopropanemethylamine (2), cyclohexylamine (3), pyrrolidine (4) cyclohexanol (5), cyclopropylmethanol (6). The structures of the novel compounds (7-17) were characterized by elemental analysis, mass spectrometry, ¹H and ³¹P NMR spectroscopy. The molecular structures of 8, 12 and 13 were determined by X-ray crystallography. The structures of all these three compounds are in the monoclinic crystal system; compounds 8 and 12 have the P21/c space group while compound 13 has the P21/n space group. The ring conformation of the cyclotriphosphazene and other external rings were investigated based on the X-ray crystal structures.