Microwave initiated synthesis and application of polyacrylic acid grafted carboxymethyl cellulose

An environmentally benign and efficient route of synthesis of polyacrylic acid grafted carboxymethyl cellulose (CMC-g-PAA) is developed using microwave radiation alone to initiate the grafting reaction. The synthesis is optimized in terms of percentage grafting and intrinsic viscosity, by varying the microwave irradiation time and monomer (acrylic acid) concentration. The grafted product has been characterized by various physicochemical characterization techniques (intrinsic viscosity measurement, FTIR spectroscopy, SEM morphology study and elemental analysis). FTIR spectroscopy confirmed that free radicals are formed on polysaccharide backbone by cleavage of 1°-OH bond, indicating microwave effect and not thermal decomposition as the cause of free radical generation. The application of the grafted product as flocculant for river water clarification, towards augmentation of drinking water supply has been investigated.     

Microwave initiated synthesis of polyacrylamide grafted Psyllium and its application as a flocculant

This paper reports a novel microwave initiated method for synthesis of polyacrylamide grafted Psyllium (Psy-g-PAM). Psyllium was modified through grafting of polyacrylamide (PAM) chains on it using microwave radiations only, in absence of any other free radical initiator. The grafting was confirmed by intrinsic viscosity study and characterization techniques like FTIR spectroscopy, elemental analysis (C, H, N, O and S) and SEM morphology study. Further, the flocculation efficacy of the synthesized graft copolymers was studied in kaolin and coal fine suspension through standard 'Jar test' procedure.     

Microwave initiated synthesis of polyacrylamide grafted carboxymethylstarch (CMS-g-PAM): Application as a novel matrix for sustained drug release

This paper reports the investigation of microwave initiated synthesized polyacrylamide grafted carboxymethylstarch (CMS-g-PAM) as matrix for sustained drug release. ‘In vitro’ release of a model drug (5-amino salicylic acid) from CMS-g-PAM matrix has been studied. It is evident that higher the percentage grafting, more sustained is the rate of drug release. Further, the percentage grafting vs. t₅₀ value (i.e. time taken for release of 50% of the enclosed drug) correlation has been successfully studied for the first time. This correlation will lead to the possibility of a programmable drug release matrix based on grafted polysaccharide. In this matrix, the rate of release of the enclosed drug can be precisely programmed simply by adjustment of percentage grafting during synthesis.     

Microwave assisted synthesis of polyacrylamide grafted starch (St-g-PAM) and its applicability as flocculant for water treatment

Polyacrylamide grafted starch (St-g-PAM) was made by a novel method of synthesis, involving combination of microwave radiation and a chemical free radical initiator (ceric ammonium nitrate) to initiate grafting reaction. This method (microwave assisted synthesis) is quick, highly reliable, reproducible and yields high quality product as compared to the conventional method (which uses a chemical free radical initiator alone to initiate the grafting reaction).The St-g-PAM grades synthesized were characterized by various physicochemical techniques. Further, its application as flocculant for wastewater treatment was investigated.     

Microwave assisted synthesis of polyacrylamide grafted agar (Ag-g-PAM) and its application as flocculant for wastewater treatment

Grafting of polyacrylamide (PAM) chains was performed onto the backbone of Agar by microwave assisted method, using microwave radiation in synergism with ceric ammonium nitrate (CAN) as the chemical free radical initiator. The intended grafting of the PAM chains were confirmed through intrinsic viscosity study, FTIR spectroscopy and elemental analysis (C, H, N, O & S). Further characterization of the grafted product was done in form of SEM morphology and TGA study. Flocculation efficacy of the synthesized graft copolymers was studied in kaolin suspension, through ‘Jar test’ procedure. Further, flocculation efficacy of the ‘best grade’ (as determined by ‘jar test’ in kaolin suspension) in wastewater was studied for possible application in reduction of pollutant load of wastewater.     

Purification of guar gum for biological applications

Commercial guar gum (GG) was purified by four different methods and characterized by gel permeation chromatography (GPC), thermogravimetric analysis and the determination of monosaccharides composition, protein and copper content, turbidity, intrinsic viscosity and rheological parameters. The first method was based on enzymatic hydrolysis with porcine pancreatin. In the second method successive gum dissolution, centrifugation and precipitation with acetone and ethanol were carried out. Precipitation with Fehling solution was employed in the third method. In the fourth method, the gum was purified by method 2 and then by method 3. All methods led to a reduction in protein content, arabinose and glucose residues, considered as sugar contaminants, and also in intrinsic viscosity and molar mass. Total elimination of protein was only achieved by method 4. Using methods 3 and 4, the gum was contaminated with small amounts of Cu(II) from the Fehling solution. Methods 2 and 4 apparently provided purer guar gum. If the amount of protein is a crucial parameter in the biological application and the guar will be taken in low amounts, method 4 is recommended. Taking into account the purity, thermal stability, rheological parameters of the purified gum and also the cost and simplicity of the procedure, method 2 has wider biological application.     

Silicone grafted bioactive peptides and their applications

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Graft copolymerization of acrylic acid onto guar gum initiated by vanadium (V)–mercaptosuccinic acid redox pair

Guar gum has been modified by graft copolymerization with acrylic acid in aqueous medium using vanadium (V)–mercaptosuccinic acid redox system. The optimum reaction conditions affording maximum grafting ratio, efficiency, add on and conversion have been determined. The grafting parameters have been found to increase with increase in vanadium (V) concentration upto 1.0 × 10⁻² mol dm⁻³, but these parameters decrease on further increasing the vanadium (V) concentration. On increasing the mercaptosuccinic acid concentration from 1.0 × 10⁻² to 4.0 × 10⁻² mol dm⁻³ grafting ratio, efficiency and add on increase up to 2.0 × 10⁻² mol dm⁻³ but decrease with further increase in mercaptosuccinic acid concentration. On varying the acrylic acid concentration from 5.0 × 10⁻² to 30.0 × 10⁻² mol dm⁻³, maximum grafting ratio, efficiency and add on have been obtained at 20.0 × 10⁻² mol dm⁻³. The grafting ratio, add on and conversion increase, on increasing the H⁺ ion concentration from 1.5 × 10⁻¹ to 6.0 × 10⁻¹ mol dm⁻³. On increasing the guar gum concentration the grafting parameters increase. The grafting ratio, add on and conversion have been found to increase with time period while efficiency started decreasing after 120 min. It has been observed that %G increases on increasing the temperature up to 35 °C. The graft copolymer has been characterized by IR spectroscopy and thermogravimetric analysis.     

Design and synthesis of new piperidone grafted acetylcholinesterase inhibitors

Alzheimer’s disease (AD) is a neurodegenerative disorder affecting 35 million people worldwide. A common strategy to improve the well-being of AD patients consists on the inhibition of acetylcholinesterase with the concomitant increase of the neurotransmitter acetylcholine at cholinergic synapses. Two series of unreported N-benzylpiperidines 5(a–h) and thiazolopyrimidines 9(a–q) molecules were synthesized and evaluated in vitro for their acetylcholinesterase (AChE) inhibitory activities. Among the newly synthesized compounds, 5h, 9h, 9j, and 9p displayed higher AChE enzyme inhibitory activities than the standard drug, galantamine, with IC₅₀ values of 0.83, 0.98, and 0.73 μM, respectively. Cytotoxicity studies of 5h, 9h, 9j, 9n and 9p on human neuroblastoma cells SH-SY5Y, showed no toxicity up to 40 μM concentration. Molecular docking simulations of the active compounds 5h and 9p disclosed the crucial role of π-π-stacking in their binding interaction to the active site AChE enzyme. The presented compounds have potential as AChE inhibitors and potential AD drugs.     

Solid-phase synthesis and applications of N-(S-acetylmercaptoacetyl) peptides

The reagent pentafluorophenyl S-acetylmercaptoacetate was used to modify the N-terminus of resin-bound side-chain-protected peptides. The modification was carried out in an automated cycle in the final stage of fluorenylmethoxycarbonyl (Fmoc)/polyamide-mediated solid-phase synthesis. Side-chain deprotection and cleavage from the resin with aqueous trifluoroacetic acid gave the N-(S-acetylmercaptoacetyl) peptides. The S-acetylmercaptoacetyl peptides were transformed into reactive thiol-containing peptides by incubation with hydroxylamine at neutral pH. The S-deacetylation was performed in the presence of a sulfhydryl-reactive compound (or intramolecular group) to enable immediate capture of the sensitive thiol. Three applications were investigated. An S-acetylmercaptoacetyl peptide, containing a sequence of a meningococcal membrane protein, was incubated with hydroxylamine in the presence of 5-(iodoacetamido)fluorescein to give the corresponding fluorescein-labeled peptide in 62% yield. The same peptide was also S-deacetylated in the presence of bromoacetylated poly-L-lysine to afford a peptide/polylysine conjugate. Finally, a peptide corresponding to a sequence of herpes simplex virus glycoprotein D was prepared. This peptide, containing an N-terminal-S-acetylmercaptoacetyl group and an additional C-terminal S-(3-nitro-2-pyridinesulfenyl)cysteine residue, was converted into a cyclic disulfide peptide (20%).     

Cyclopentadienylcobalt sulfide and selenide cluster compounds: synthesis and structural characterizations

The reaction of CpCo(CO)₂ with elemental sulfur yielded the new sulfur-rich compound Cp₄Co₄(μ₃-S)(μ₃-S₂)₃ (1). The structure of 1 contains a Co₄S₇ core composed of three μ₃-disulfido ligands and one μ₃-sulfido ligand. PEt₃ abstracts sulfur from 1 to yield the new compound Cp₄Co₄(μ₃-S)₃(μ₃-S₂) (2). Compound 2 is also a cage compound, but it contains three μ₃-sulfido ligands and only one μ₃-disulfido ligand. Compound 2 is converted back to 1 by reaction with elemental sulfur. The selenium homologue Cp₄Co₄(μ₃-Se)₃(μ₃-Se₂) (3) was obtained from the reaction of CpCo(CO)₂ with elemental selenium. The structures of 1, 2 and 3 were determined by single-crystal X-ray diffraction analyses.     

HTHQ (1-O-hexyl-2,3,5-trimethylhydroquinone), an anti-lipid-peroxidative compound: its chemical and biochemical characterizations

Recently, it has become apparent that reactive oxygen species (ROS) play many important roles in biological systems. For example, relationships between many diseases, such as cancer, cardiac infarction and arteriosclerosis, and ROS have been found. It is also well known that anti-oxidative agents scavenge ROS in biological systems, which in turn prevents ROS-related diseases. In our previous efforts to develop effective anti-oxidative compounds, we found that 1-O-hexyl-2,3,5-trimethylhydroquinone (HTHQ), which is a hydroquinone monoalkyl ether, is a potent anti-oxidative agent. Here, the scavenging activities of HTHQ against ROS, such as superoxide anion radicals, hydroxyl radicals, t-butyl peroxyl radicals and singlet oxygens, were examined by the ESR (electron spin resonance)-spin trapping method. Among ROS, HTHQ scavenged t-butyl peroxyl radicals most effectively (IC₅₀=0.31±0.04 mM), showing approximately twice the activity of a well-known lipophilic anti-oxidant, d,l-α-tocopherol (IC₅₀=0.67±0.06 mM), as measured by IC₅₀ values defined as the 50% inhibition concentration of the generated ROS. In addition, a relatively stable ESR spectrum of free radicals due to HTHQ was observed during the reaction of HTHQ and t-butyl peroxyl radicals, indicating a direct reaction of HTHQ and t-butyl peroxyl radicals. The free radicals due to HTHQ were more stable than those derived from d,l-α-tocopherol under the same conditions examined. On the basis of these results, we evaluated anti-lipid-peroxidative activity of HTHQ in three systems involving micelles, liposomes and rat liver microsomes. HTHQ exhibited a similar anti-oxidative activity to that of d,l-α-tocopherol against lipid peroxidation in linolate micelles initiated by addition of Fe²⁺. On the other hand, HTHQ exhibited approximately 4.8-fold higher anti-lipid-peroxidation activity than that of d,l-α-tocopherol against the peroxidation in phosphatidylcholine liposomes initiated by addition of Fe²⁺. Furthermore, HTHQ scavenged the lipid peroxides at a rate approximately 150 times higher than that of d,l-α-tocopherol against Fe³⁺-ADP-induced lipid peroxidation in rat liver microsomes, indicating that the anti-lipid-peroxidation activity of HTHQ might be substantially elevated in biological systems in comparison with that of d,l-α-tocopherol. Based on these results, we suggest that HTHQ reacts directly with peroxyl radicals, such as t-butyl peroxyl radicals and peroxides of linolate micelles, liposomes and microsomes, by scavenging them to form stable free radicals. The resulting free radicals are presumed to be reduced by several reducing mechanisms in biological systems similarly to those of d,l-α-tocopherol, and then the lipid-peroxidation reactions will be terminated. In conclusion, HTHQ was found to be a potent anti-lipid-peroxidative compound and its anti-oxidation activity to be extremely elevated in biological systems, such as that of liver microsomes via the generation of stable free radicals. We propose that HTHQ is a potent anti-oxidative agent for use in future treatments for lipid-peroxide relevant diseases.     

Sustainable synthesis and applications of polyhydroxyalkanoates (PHAs) from biomass

Polyhydroxyalkanoates (PHAs) belong to group of biopolymers that have in recent times received growing research interest as a result of being eco-friendly and close characteristics with petrochemical based plastics. Alternatives to utilization of synthetic plastics are being explored since synthetic plastics are non-recyclable and non-biodegradable in nature. One of the innovations of Green Chemistry is utilization of renewable feedstocks such as biomass to achieve sustainable development with future circular economy. Bio-based products are of great interest to sustainable development as a result of diminishing fossil fuel reserves and rising environmental concerns. This review summarizes the productions of PHAs from renewable feedstocks such as lignocellulose, crude glycerol, levulinic acid (LA), palm-oil mill effluents (POME) and waste oils. The production of bio-based polymers has become much more professional and differentiated in recent years. Presently, there are bio-based alternatives for practically every application, therefore, this review presents applications of PHA in bio-refinery, medical sectors, agriculture sector, construction industry, and in packaging industry. The cost analysis of PHA from renewable sources with commercially available ones and potential to attain circular economy were also stressed. The reasons for this shift are connected to the non-renewability of fossil-based resources, the deteriorating environmental impacts, and the lack of biodegradability of the petroleum-produced materials.     

Microbial synthesis of poly(epsilon-lysine) and its various applications

This review article deals with the microbial synthesis, physiochemical properties, and potential applications of poly-epsilon-lysine (epsilon-PL), which is a naturally occurring biomaterial that is water soluble, biodegradable, edible and non-toxic toward humans and the environment. The potential applications of epsilon-PL as food preservatives, emulsifying agent, dietary agent, biodegradable fibers, highly water absorbable hydrogels, drug carriers, anticancer agent enhancer, biochip coatings in the fields of food, medicine, agriculture and electronics are also discussed in this review.     

Polyacrylamide grafted Agar: Synthesis and applications of conventional and microwave assisted technique

Polyacrylamide grafted Agar (Ag-g-PAM) has been successfully synthesized by conventional method and microwave assisted method. The former method employs ceric ammonium nitrate (CAN) as the free radical initiator while the latter uses the combination of ceric ammonium nitrate (CAN) and microwave irradiation. The synthesized graft copolymers have been characterized by elemental analysis (C, H, N, O and S), FTIR spectroscopy, intrinsic viscosity measurement and scanning electron micrograph (SEM); taking agar as a reference. Flocculation efficacy of synthesized graft copolymers was studied in kaolin suspension and in waste water through 'Jar test' procedure. In the present investigation, we have observed that polyacrylamide grafted agar synthesized by microwave assisted technique shows superior properties than conventional technique. These properties are reported in terms of intrinsic viscosity, flocculation efficacy and pollutant load reduction of waste water.     

DNA合成技术及应用

DNA从头合成技术是指以寡核苷酸链为起始的合成DNA片段的技术,其不断进步是合成生物学快速发展的基石之一。常规使用的连接介导的DNA合成技术和PCR介导的DNA合成技术日益成熟,精确合成长度已经达到0．5—1kb。微阵列介导的DNA合成技术不断发展,其低成本、高通量的特点吸引了人们的注意;而酵母体内DNA合成技术的成功探索也为体外DNA合成提供了一种补偿方法。DNA合成在优化密码子用于异源表达、构建异源代谢途径、合成人工基因组以及合成减毒病毒用于疫苗研制等方面有广泛应用。综述了DNA从头合成技术的研究进展,并介绍了DNA合成的前沿应用。     

Rheological properties of guar gum and hydroxyethyl guar gum in aqueous solution

The rheological properties of aqueous solutions of guar gum (GG) and hydroxyethyl guar gum (HEG) have been investigated. The flow properties of these polysaccharide solutions were studied at the shear rate in the range 1.5–1310s⁻¹ using a Rheotest-2 viscometer. The flow of these polysaccharide solutions was described by equation of state based on Cross model. The basic rheological parameters, like zero shear rate viscosity (η_o), elasticity modulus (G_o) and relaxation time (gl_o) were calculated using simple and established relations. Master viscosity curves indicated that the molecular weight distribution of native guar gum has been changed by hydroxyethylation under specified reaction conditions. The effect of concentration and temperature on η_o and λ_o has been studied, and the relations among these were established by simple equations.     

Composite boards from guar and sorghum (Dura) stalks

Laboratory trials were carried out to determine the suitability of guar and sorghum stalks from Sudan as basic materials for composite insulation boards manufacture using cement as binder. Lignocellulosic material-to-cement ratios of 1:15 and 1:2 were used. The results show that these raw materials could successfully be used for insulation boards, with density of 530–700 kg/m³, satisfactory strength, and very good heat-insulation properties making them suitable for building.