Inside-Needle Extraction Method Based on Molecularly Imprinted Polymer for Solid-Phase Dynamic Extraction and Preconcentration of Triazine Herbicides Followed by GC–FID Determination

An inside-needle extraction method was developed through thermal polymerization of atrazine-molecularly imprinted polymer (MIP) on the internal surface of a stainless steel hollow needle, which was oxidized and silylated. The fabricated coating (MIP layer) for the needle was durable and showed very good chemical and thermal stability. It could be mounted on a glass syringe and be directly coupled with gas chromatographic (GC) systems. The parameters being effective on the coating and extraction processes, namely nature of oxidizing agent, silylation time, nature and amount of porogen, template-to-MIP components ratio, polymerization time and temperature, sample volume, flow rate, pH and ionic strength of the sample were investigated and optimized. The extraction needle showed high selectivity as well as a great extraction capacity for triazines. The extraction of atrazine, simazine, cyanazine, ametryn, prometryn and terbutryn using the fabricated extraction needle and followed by GC analysis resulted in detection limits of 2.6, 21, 24, 32, 38 and 42 ng mL⁻¹, respectively. The fabricated needle proved to be applicable to the analysis of real samples by comparing the results obtained for non-spiked and spiked samples of grape juice, tap water and groundwater.

     

An investigation of Forex market efficiency based on detrended fluctuation analysis: A case study for Iran

The efficient market hypothesis (EMH) states that asset prices fully reflect all available information. As a result, speculators cannot predict the future behavior of asset prices and earn excess profits at least after adjusting for risk. Although initial tests of the EMH were performed on stock market data, the EMH was soon applied to other markets including foreign exchange (FX). This study uses the detrended fluctuation analysis (DFA) technique to test 01:12:2005–18:04:2010 Iranian Rial/US Dollar exchange rate time series data to see if it can be explained by the weak form of the EMH. Moreover, to determine changes in the degree of inefficiency over time, the whole period has been divided into four subperiods. The study shows that the Iranian Forex market (the Rial/Dollar case) is weak-form inefficient over the whole period and in each of the subperiods. However, the degree of inefficiency is not constant over time. The findings suggest that profitable risk-adjusted trades could be made using past data.     

Synthesis and characterization of A2 + B3 type hyperbranched aromatic-aliphatic polyester with carboxyl end groups

New types of carboxyl-terminated hyperbranched polyesters (HBPEs) with aromatic-aliphatic structure were synthesized by single step-melt polycondensation of adipic acid (as A2 monomer) and phloroglucinol (as B3 monomer) as a core via A₂ + B₃ approach, at three different monomer mole ratios (A₂/B₃ = 1: 1, 1.5: 1, 2: 1, respectively). FTIR spectroscopy indicated that the polymers contained hydroxyl groups, ester bonds, benzene ring, methyl and methylene groups, which were in agreement with the expected HBPEs. The HBPEs have inherent viscosities about 0.24 to 0.27 dL/g. The degree of branching of the HBPEs was estimated to be 0.45–0.49% by ¹H-NMR and ¹³C-NMR measurements. The melting temperature of HBPE-1, HBPE-2 and HBPE-3 were 154, 155 and 160°C respectively measured by differential scanning calorimetry (DSC). The synthesized polymers were thermally stable; the thermogravimetric analysis (TGA) measurement revealed that HBPEs had 10% weight loss at 310°C in nitrogen.     

Improvement of Nanoprecipitation Technique for Preparation of Gelatin Nanoparticles and Potential Macromolecular Drug Loading

An optimum nanoprecipitation technique for gelatin nanoparticles is established, based on aqueous gelatin solution and ethanolic solution containing stabilizer. Crosslinking with glutaraldehyde results in stable gelatine nanoparticles. Several factors such as the surfactant concentration, type of surfactant, type of nonsolvent and gelatin concentration are evaluated. Gelatin nanoparticles with 200–300 nm can be produced using 20–30 mg mL^?1 of gelatin and a minimum of 7% w/v stabilizer (Poloxamer 407 or 188). Furthermore, methanol and ethanol are good nonsolvents, whereas other nonsolvents such as acetone, isopropyl alcohol, and acetonitrile, result in phase separation and visible precipitates. The entrapment efficiency of fluorescein‐isothiocyanate (FITC)‐dextran as model drug was determined to 50% with no substantial effect on particle size. 80% of the drug is only released after enzymatic digestion.

     

Convenient Synthesis of 2-Aminothiophene Derivatives by Acceleration of Gewald Reaction Under Ultrasonic Aqueous Conditions

Under ultrasound irradiation and in the presence of H₂O/Et₂NH, ethyl cyanoacetate or malononitrile can combine with α-methylene carbonyl compounds and elemental sulfur to efficiently yield 2-aminothiophene derivatives within a few minutes. Products are easily obtained by simple filtration because of their spontaneous precipitation in the reaction mixtures.     

One-Pot,Three-Component Coupling Reaction: Catalyst-Free Green Synthesis of Novel N-Heteroaryl α-Naphthylglycines

A series of novel N-heteroaryl α-arylglycines containing naphthol rings has been prepared by one-pot, three-component condensation reaction of glyoxalic acid, heteroaryl amines and naphthols in water at ambient temperature and under reflux conditions in moderate to high yields. The promising advantages such as removal of organic solvent, no need to catalyst, simplicity of the reaction procedure and easy product separation will be discussed in this article.     

Diammonium Hydrogen Phosphate: An Efficient and Versatile Catalyst for the One‐Pot Synthesis of Tetrahydrobenzo[b]pyran Derivatives in Aqueous Media

Diammonium hydrogen phosphate was used as a mild, efficient, neutral, and cheap catalyst for the synthesis of various 4H‐benzo[b]pyran derivatives via a one‐pot, three‐component condensation of aromatic aldehydes, active methylene compounds, and dimedone in aqueous media.     

Characterization of Chitosan/Alginate Self-Assembled Nanoparticles as a Protein Carrier

The aim of this study was to evaluate the effect of the polymeric ratios on the characteristics of chitosan/alginate (ch/alg) self-assembled nanoparticles and their potential as protein delivery vehicle. The nanoparticles were prepared using proper mixing of polymers in presence or absence of bovine serum albumin (BSA) as a protein model. Three formulations of nanoparticles comprising ch/alg ratios of 2:1, 1:1, and 1:2 were prepared. Size, shape and zeta potential of the formulations were studied by scanning electron microscopy (SEM) and nanosizer instruments. FTIR, and differential scanning calorimetery (DSC) studies were performed to investigate polymer-polymer or polymer-protein interactions. Release profiles and entrapment efficiencies of the nanoparticles were determined by calorimetric technique using appropriate techniques. Entrapment efficiency was 70% for ch/alg ratio of 1:1, 65% for 1:2, and 60% for 2:1. The z-average size of the nanoparticles were 403, 205, and 318 nm for ch/alg ratios of 2:1, 1:1, and 1:2, respectively. Average zeta potentials were ?47, +15, ?25 mV for 2:1, 1:1, and 1:2 as well. Considering the favorable features required for protein delivery systems, ch/alg (1:1) due to its smallest size, highest loading, and most homogenous shape was regarded as the best ratio.     

In Silico and Experimental Characterization of Chimeric Bacillus thermocatenulatus Lipase with the Complete Conserved Pentapeptide of Candida rugosa Lipase

Lipases are one of the highest value commercial enzymes as they have broad applications in detergent, food, pharmaceutical, and dairy industries. To provide chimeric Bacillus thermocatenulatus lipase (BTL2), the completely conserved pentapeptide (¹¹²Ala-His-Ser-Gln-Gly¹¹⁶) was replaced with similar sequences (²⁰⁷Gly-Glu-Ser-Ala-Gly²¹¹) of Candida rugosa lipase (CLR) at the nucleophilic elbow region. For this purpose, three mutations including A112G, H113E, and Q115A were inserted in the conserved pentapeptide sequence of btl2 gene. Based on the crystal structures of 2W22, the best structure of opened form of the chimeric lipases were garnered using the MODELLER v9.10 software. The native and chimeric lipases were docked to a set of ligands, and a trial version of Molegro Virtual Docker (MVD) software was used to obtain the energy values. Docking results confirmed chimeric lipase to be better than the native lipase. Following the in silico study, cloning experiments were conducted and expression of native and chimeric btl2 gene in Pichia pastoris was performed. The native and chimeric lipases were purified, and the effect of these mutations on characteristics of chimeric lipase studied and then compared with those of native lipase. Chimeric lipase exhibited 1.6-fold higher activity than the native lipase at 55 °C. The highest percentage of both lipases activity was observed at 60 °C and pH of 8.0. The ion Ca²⁺ slightly inhibited the activity of both lipases, whereas the organic solvent enhanced the lipase stability of chimeric lipase as compared with the native lipase. According to the results, the presence of two glycine residues at the conserved pentapeptide region of this chimeric lipase (¹¹² Gly-Glu-Ser-Ala-Gly ¹¹⁶) may increase the flexibility of the nucleophilic elbow region and affect the enzyme activity level.