Simultaneous determination of bromoxynil and MCPA in commercial samples and raw materials using reversed phase high performance liquid chromatography.

This study encompasses a quick, efficient, repeatable and reproducible analytical method for simultaneous determination of Bromoxynil (3, 5-Dibromo-4-hydroxybenzonitrile) and MCPA (2-methyl-4-chlorophenoxyacetic acid) using RP-HPLC with UV-Detector. Bromoxynil + MCPA is one of the most selective post emergent herbicide formulations for the control of important broad leaf weeds infesting small grains (wheat, barley, oats, rye), conservation reserve program areas and grass grown for seed. Optimum weed control is achieved when Bromoxynil + MCPA is applied to actively growing weed seedlings. So, a simple, repeatable, reproducible and efficient simultaneous analytical method was developed for Bromoxynil + MCPA. The developed method was applied for the detection and quantitation of these pesticides in formulations and raw materials with excellent recoveries. It was validated according to ICH Guidelines with excellent linearity R2 = 0.992 for Bromoxynil and 0.998 for MCPA. For Bromoxynil, LOD = 1.57 mg/L and LOQ = 5.22 mg/L while for MCPA the LOD = 1.08 mg/L and LOQ = 3.62 mg/L was found. The proposed method has shown high precision (RSD %) 0.06% and 0.11% for Bromoxynil and MCPA respectively while the trueness has been calculated in terms of recovery percentage obtained as "mean value of Bromoxynil 99.53% and MCPA 100.10%" which is excellent under optimized conditions. For repeatability and reproducibility, five replicate readings of standard and sample were taken and had found within acceptable limits of relative standard deviation (RSD ≤ ± 2%). Finally, the robustness of the developed method was determined by changing flow rate and mobile phase ratios that has found within the permissible limits (% RSD NMT 1.5). So, the proposed analytical method has found to be more precise, valid and accurate at commercial scale.

Fundamentals and Design-Led Synthesis of Emulsion-Templated Porous Materials for Environmental Applications.

Emulsion templating is at the forefront of producing a wide array of porous materials that offers interconnected porous structure, easy permeability, homogeneous flow-through, high diffusion rates, convective mass transfer, and direct accessibility to interact with atoms/ions/molecules throughout the exterior and interior of the bulk. These interesting features together with easily available ingredients, facile preparation methods, flexible pore-size tuning protocols, controlled surface modification strategies, good physicochemical and dimensional stability, lightweight, convenient processing and subsequent recovery, superior pollutants remediation/monitoring performance, and decent recyclability underscore the benchmark potential of the emulsion-templated porous materials in large-scale practical environmental applications. To this end, many research breakthroughs in emulsion templating technique witnessed by the recent achievements have been widely unfolded and currently being extensively explored to address many of the environmental challenges. Taking into account the burgeoning progress of the emulsion-templated porous materials in the environmental field, this review article provides a conceptual overview of emulsions and emulsion templating technique, sums up the general procedures to design and fabricate many state-of-the-art emulsion-templated porous materials, and presents a critical overview of their marked momentum in adsorption, separation, disinfection, catalysis/degradation, capture, and sensing of the inorganic, organic and biological contaminants in water and air.

Antiviral activity of hexapeptides derived from conserved regions of bacterial proteases against HCV NS3 protease.

The main cause of hepatitis C is hepatitis C virus or HCV and for the cure of hepatitis C, NS3/4A protease has been found an important and emerging target. A number of HCV NS3/4A protease inhibitors have been discovered which have shown subsequent reduction in reducing the viral load leading to this infection however they are still undergoing clinical trials for improvement. Bacterial proteases are of great pharmaceutical importance and have a key role in various biological processes and in life cycle of several pathogens. The current study was planned to explore hexapeptides derived from conserved regions of bacterial proteases for their potential in blocking the NS3 protease activity of HCV which would finally inhibit HCV multiplication. For this, a novel protease gene nprB was isolated from a thermophilic bacterium Streptomyces thermovulgaris and bioinformatics analyses were performed. PCR amplification and sequencing of nprB gene indicated an open reading frame of 178 aa (20191.18 Dalton).The peptide GGVHIN was the top ranked with minimum S-score of -17.21) followed by hexapeptides VDAHAN, GVGREA, GALNES and VHINSS with their S-scores of -14.73, -13.78, -10.72 and -10.70, respectively. A phylogram was also reconstructed to reveal evolutionary relationships of nprB with its various homologs. The provided data will serve as a background to further reveal pharmaceutical and biotechnological importance of this novel protease gene from S. thermovulgaris in future.

Hyperbranched Polyethylenimine-Tethered Multiple Emulsion-Templated Hierarchically Macroporous Poly(acrylic acid)-Al2O3 Nanocomposite Beads for Water Purification.

Emulsion template-guided strategy has been used to produce porous architectures with exquisite structure, tailored morphology, and exclusive features for ubiquitous applications. Notwithstanding, the practical water remediation is often marred by their transport-limited behavior and fragility. To circumvent these conundrums, we prepared hierarchically porous poly(acrylic acid)-alumina nanocomposite beads by solidifying the droplets of emulsions jointly stabilized by the organic surfactants and alumina nanoparticles. By virtue of their positive charge, the alumina nanoparticles got entrapped within the poly(acrylic acid) scaffolds that excluded the risk of secondary contamination typically observed with conventional nanocomposites. Being amenable to surface modification, the carboxyl moieties of the beaded polymer were further exploited to covalently tether branched polyethylenimine throughout the exterior and interior surface of the porous matrix via a grafting-to approach. The macropores expedite an active fluid flow and easier adsorbate transport throughout the functionalized nanocomposites whose overall higher density of positive charge over a certain pH range electrostatically attracts and effectively adsorbs the negatively charged Cr(VI) complexes and anionic congo red ions/molecules from water. This proof-of-concept synthetic approach and postsynthetic modification offer an improved mechanical robustness to these macrosized multifunctional nanocomposite beads for their easier processing, thereby paving the way for the point-of-use water purification technology development.

Extraction of Metronidazole and Furazolidone from industrial effluents by double salting out assisted liquid liquid extraction technique and their analyses by HPLC-UV method.

We have developed a new analytical method for simultaneous determination of Metronidazole and Furazolidone by High Performance Liquid Chromatography (HPLC). The method is coupled to double salting-out assisted liquid-liquid extraction (SALLE) which facilitates the detection and quantification of Metronidazole and Furazolidone in different dosage forms by subsequent HPLC analysis. Extraction parameters such as solvent, pH and salt concentration are optimized and liquid liquid extraction showed efficiency up to 102% and 100% for Metronidazole and Furazolidone respectively in chloroform, at pH 3 and low salt concentration (0.5g KCl and 0.5 gNaNO3). The designed simultaneous analytical method is further validated and Metronidazole and Furazolidone showed linearity upto R20.994 and 0.9936 respectively. LOD was 2.1µg/ml, 1.5µg/ml and LOQ was 21.1µg/ml, 15.2µg/ml for metronidazole benzoate and furazolidone. Precision of the method is 1.84% (RSD) and 1.72% (RSD) for Metronidazole and Furazolidine respectively. Moreover, accuracy is measured in terms of percent recovery which is more than 100% for both analytes under optimized conditions. Finally, robustness is evaluated by changing the flow rate and detection wavelength which is also obtained within permissible limit. This indicates that the proposed method is simple, efficient and shows excellent recoveries for simultaneous determination of Metronidazole and Furazolidone in different dosage forms and Industrial effluents.

Isolation and characterization of nprB, a novel protease from Streptomyces thermovulgaris.

Bacterial proteases are of great pharmaceutical importance and have a key role in various biological processes and in life cycle of several pathogens. New technology used for rational protein engineering as well improved delivery options will expand the potential pharmaceutical applications of proteases. The catalytic proteases belong to metalloproteases (EC.3.4.24) that comprise thermo lysine. The metalloproteases and their homologs have many important biotechnological and therapeutic applications. In the present study, a novel protease gene nprB was isolated from a thermophilic bacterium Streptomyces thermovulgaris and bioinformatics analyses were performed. PCR amplification and sequencing of nprB gene indicated an open reading frame of 178 aa (20191.18 Dalton). Based on protein sequence homology as well as conserved motifs and PTF domain the protein is characterized as a thermo lysine-like protease and is a member of M4 family of metalloproteases. Different bioinformatics tools such as ProtParam, SOPMA, signalP4.1 and ProDom from the ExPAsy server were used for structural and functional analyses. A phylogram was also reconstructed to reveal evolutionary relationships of nprB with its various homologs. The provided data will serve as a background to further reveal pharmaceutical and biotechnological importance of this novel protease gene from S. thermovulgaris in future.

Fabrication of Emulsion-Templated Poly(vinylsulfonic acid)-Ag Nanocomposite Beads with Hierarchical Multimodal Porosity for Water Cleanup.

Emulsion templating has emerged as a cutting-edge technique to prepare a wide array of porous polymer-metal nanocomposites with intriguing properties. Using this strategy, we set out to prepare novel hierarchically porous poly(vinylsulfonic acid) beads, which were then used for the in situ production of silver nanoparticles to obtain poly(vinylsulfonic acid)-Ag nanocomposite beads via a facile approach. Owing to their multimodal macro-meso-/microporosity that accounts for their decent BET surface areas (170.75-197.74 m2/g) and easier mass diffusion and transport together with the synergistic benefits of very small silver nanoparticles (down to ∼3.77 nm), the nanocomposite beads are found effective to remove Hg(II) and RhB and to kill Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive) bacteria. The adsorption capacities (167.98-190.58 mg/g) of these materials for Hg(II) surpass some recently reported benchmark materials. The larger size (1.56 ± 0.20-1.50 ± 0.14 mm) of the beads that helps favor the handling and subsequent recovery for recycling is also very useful to further broaden the horizons of these materials to develop decentralized water treatment systems.

Magnetic Hierarchically Macroporous Emulsion-Templated Poly(acrylic acid)-Iron Oxide Nanocomposite Beads for Water Remediation.

Tainting of waterbodies with noxious industrial waste is the gravest environmental concern of the day that continues to wreak inevitable havoc on human health. To cleanup these hard-to-remove life-threatening water contaminants, we have prepared hierarchically porous poly(acrylic acid) beads by emulsion templating. These emulsion-templated macroporous polymer beads not only mediate the synthesis of Fe3O4 nanoparticles inside their porous network using a coprecipitation approach but, in turn, create diverse anchoring sites to immobilize an additional poly(acrylic acid) active layer onto the nanocomposite beads. These post-synthetically modified nanocomposite beads with macropores and abundant acrylic acid moieties offer the ready mass transfer and fair advantage of relatively higher overall negative charge to efficiently adsorb lead [Pb(II)] and crystal violet with impressive performance-even superior to many of the materials explored in this regard so far. Furthermore, the strong entanglement of nanoparticles in the porous polymeric scaffolds tackles the curb of trade-off between all-round effective remediation and secondary pollution and the millimeter size eases their processing and recovery during the adsorption tests, thereby making these materials practically worthwhile.

A novel spectrophotometric determination of caroverine in pharmaceutical formulations via derivatization with Folin-ciocalteu Phenol reagent.

In this study we have reported a new, fast and extraction free spectrophotometric procedure for the assessment of caroverine in pharmaceutical raw and tablet dosage forms. In the reported visible spectrophotometric procedure tungstate in Folin-Ciocalteu phenol reagent is reduced in alkaline medium and produces the blue colored chromogen that shows Λmax at 740nm with the calibration range of 2-28µg/ml. The LOD and LOQ values are 1.15 and 3.81µg/ml respectively. The newly developed analytical procedure is used to determine caroverine in raw material of and commercial tablets dosage forms. The spectrophotometric method represented in this study is simple, rapid and extraction free. It may easily be utilized for the determination of caroverine in pharmaceutical laboratories for quality control and stability studies purpose.

Experimental investigations on a diesel engine operated with fuel blends derived from a mixture of Pakistani waste tyre oil and waste soybean oil biodiesel.

The waste tyre and waste cooking oils have a great potential to be used as alternative fuels for diesel engines. The aim of this study was to convert light fractions of pyrolysis oil derived from Pakistani waste vehicle tyres and waste soybean oil methyl esters into valuable fuel and to reduce waste disposal-associated environmental problems. In this study, the waste tyre pyrolysis liquid (light fraction) was collected from commercial tyre pyrolysis plant and biodiesel was prepared from waste soybean oil. The fuel blends (FMWO10, FMWO20, FMWO30, FMWO40 and FMWO50) were prepared from a 30:70 mixture of waste tyre pyrolysis liquid and waste soybean oil methyl esters with different proportions of mineral diesel. The mixture was named as the fuel mixture of waste oils (FMWO). FT-IR analysis of the fuel mixture was carried out using ALPHA FT-IR spectrometer. Experimental investigations on a diesel engine were carried out with various FMWO blends. It was observed that the engine fuel consumption was marginally increased and brake thermal efficiency was marginally decreased with FMWO fuel blends. FMWO10 has shown lowest NOx emissions among all the fuel blends tested. In addition, HC, CO and smoke emissions were noticeably decreased by 3.1-15.6%, 16.5-33.2%, and 1.8-4.5%, respectively, in comparison to diesel fuel, thereby qualifying the blends to be used as alternative fuel for diesel engines.

Polyacrylamide exotemplate-assisted synthesis of hierarchically porous nanostructured TiO2 macrobeads for efficient photodegradation of organic dyes and microbes.

Nano/microscale TiO2 materials and their composites have reached the pinnacle of their photocatalytic performances to destroy persistent organic pollutants and waterborne microorganisms, but their practical applications are limited by the drawbacks associated with their stability, leaching, processing and separation. To overcome these shortcomings, we have prepared hierarchically porous nanostructured TiO2 macrobeads via an exotemplating or nanocasting strategy by infiltrating the TiO2 sol into the emulsion-templated porous polyacrylamide scaffold followed by its gelation, drying and calcination. The nanoscale TiO2 building units tailor the shape of the porous polymeric network after calcination thereby retaining the macroscale morphology of polymer beads after template removal. A novel combination of the hierarchical macroporosity, orderly crystalline anatase nature, nanoscale feature and good surface area revealed by the relevant characterization tools makes these TiO2 scaffolds particularly effective for superior degradation of methylene blue with the enhanced rate constant and efficient disinfection of E. coli and S. aureus under UV light. The macrosize and mechanical stability of these purely TiO2 beaded architectures have several potential advantages over conventional TiO2 nanocomposites and slurry systems to address the inherent bottlenecks of secondary contamination, difficult operation and energy-intensive post-recovery processes that are indeed deemed to be the barriers to develop practically useful water treatment technologies.

Development of Silver-Nanoparticle-Decorated Emulsion-Templated Hierarchically Porous Poly(1-vinylimidazole) Beads for Water Treatment.

Water, the driver of nature, has always been polluted by the blind hurling of highly toxic contaminants, but human-friendly science has continuously been presenting better avenues to help solve these challenging issues. In this connection, the present study introduces novel nanocomposites composed of emulsion-templated hierarchically porous poly(1-vinylimidazole) beads loaded with the silver nanoparticles generated via an in situ approach. These nanocomposites have been thoroughly characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, Brunauer-Emmett-Teller, and field emission scanning electron microscopy. The appropriate surface chemistry, good thermal stability, swelling behavior, porosity, and nanodimensions contributed to achieve very good performance in water treatment. Owing to their easier handling and separation, these novel nanocomposites are highly efficient to remove arsenic and eriochrome black T with decent adsorption capacities in addition to the inactivation and killing of Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive) bacteria.

A Comparative Study on Hemp (Cannabis sativa) Essential Oil Extraction Using Traditional and Advanced Techniques.

A comparative study of Cannabis sativa (Hemp) essential constituents obtained by using Supercritical Fluid Extraction (SCFE), Steam Distillation (SD) and Hydrodistillation (HD) is presented here. The optimized extraction temperatures were 130，110 and 50 ℃ for hydrodistillation, steam distillation and supercritical fluid extraction respectively. The essential oil of C. sativa was analyzed by using Gas chromatography mass spectrometry (GC-MS). A total of 33, 30 and 31 components have been identified in HD, SD and SCFE respectively. Yield of essential oil using SCFE (0.039%) was more than HD (0.025%) and SD (0.035%) extraction respectively. The main component of sesquiterpenes obtained by hydrodistillation at 130 ℃ with their percentages included caryophyllene (40.58%), trans-α-bergamotene (5.41%), humulene (10.97%), cis-ß-farnesene (8.53%) and monoterpenes included α-pinene (2.13%), d-limonene (6.46%), p-cymol (0.65%) and cineole (2.58%) respectively. The main component of sesquiterpenes obtained by SD steam distillation at 110 ℃ including caryophyllene (38.60%) trans-α-bergamotene (4.22%), humulene (10.26%), cis-ß-farnesene (6.67%) and monoterpenes included α-pinene (3.21%), d-limonene (7.07%), p-cymol (2.59%) and cineole (3.88%) whereas the more percentages of major components were obtained by SCFE at 50 ℃ included caryophyllene (44.31%), trans-α-bergamotene (6.79%), humulene (11.97%) cis-ß-farnesene (9.71%) and monoterpenes included α-pinene (0.45%), d-limonene (2.13%) p-cymol (0.19%) and cineole (1.38 %) respectively. We found yield/efficiency, chemical composition, quality of the essential oils by supercritical fluid extraction superior in terms of modern, green, saving energy and a rapid approach as compared to traditional techniques.

Pharmacological investigations and Petra/Osiris/Molinspiration (POM) analyses of newly synthesized potentially bioactive organotin(IV) carboxylates.

A series of organotin(IV) carboxylate complexes: [Me2SnL2] (1), [n-Bu2SnL2] (2), [n-Oct2SnL2] (3), [Me3SnL] (4), [n-Bu3SnL] (5) and [Ph3SnL] (6), where L=3-(4-fluorophenyl)acrylic acid, have been successfully synthesized and characterized by FT-IR, NMR ((1)H, (13)C) and single crystal analysis. The ligand coordinates to tin atom via carboxylate group. Compound 4 was also analyzed by single crystal XRD analysis. Crystallographic data for trimethyltin(IV) complex showed that the tin has approximate trigonal bipyramidal geometry with the CH3 groups in the trigonal plane. The carboxylate groups bridge the adjacent tin atoms, resulting in polymeric chains. FT-IR and NMR data also support the 5-coordination geometry for the triorganotin(IV) derivatives. In the case of the diorganotin(IV) derivatives a six-coordinate geometry at the tin atom is proposed from spectroscopic data. The Me-Sn-Me bond angle in complexes 1 and 4 was determined from the (2)J[(119)Sn-(1)H] value as 138.4° and 111° that falls in the range of 5-coordinated trigonal bipyramidal and 6-coordinated octahedral geometries, respectively. The synthesized compounds were screened for their biological activities including antibacterial, antifungal and cytotoxicity. The compounds 4-6 exhibit excellent antibacterial, antifungal and cytotoxic activities. The cytotoxicity data reveals that the HL and 1-3 are almost non-toxic and exhibited LD50 values in the range 73.45-675.1µg/mL while 4-6 are found to be cytotoxic to mildly cytotoxic with LD50 values in the range 6.43-13.49µg/mL. The compound interacts with DNA via intercalation of aromatic ring into the base pairs of DNA resulting in hypochromism and minor red shift.

Spectrophotometric determination of citalopram hydrobromide in tablet dosage form using chloranil.

A fast, sensitive and extraction free spectrophotometric method for the quantitative determination of citalopram hydrobromide in pharmaceutical raw and tablet formulations has been proposed. The newly proposed method is based on the charge transfer reaction between citalopram as electron donor and chloranil as electron acceptor. The charge transfer complex of citalopram and chloranil shows λ(max) at 550 nm in methanol. The experimental conditions such as reaction time, temperature, stoichiometry of the colored complex have been optimized. The developed method allows the determination of citalopram hydrobromide over a concentration range of 1-25 mg/ ml. The proposed method is used to determine the citalopram in tablet dosage forms. The results of proposed method are compared to the official USP method. The newly developed method is accurate, reproducible and easy to perform. It does not require stringent experimental conditions. No interference has been observed for excipients and additives in tablet formulations.

Comparative evaluation of some commercially available brands of pharmaceutical preparations for Na, K and Mg concentrations.

A study was carried out to investigate the concentrations of macro-elements (Na(+), K(+) and Mg(+2)) in twelve commercially available pharmaceutical preparations used as sex stimulant, by Atomic Absorption Spectrophotometer. A wet digestion method was adopted to prepare the samples. The results indicated that sodium concentration was maximum (3702 ± 29 µg g(-1)) in LB and minimum (495 ± 06 µg g(-1)) in H-E-H. Potassium concentration was maximum (6337 ± 13 µg g(-1)) in NBA while minimum (150 ± 06 µg g(-1)) in ZGRA. Magnesium concentration was maximum in V-100 (9226 ± 11 µg g(-1)) and minimum in FGRA (1194 ± 25 µg g(-1)). The concentration of macro-elements in the imported herbal preparations was in the order of Mg

Immobilization of Rose Waste Biomass for Uptake of Pb(II) from Aqueous Solutions.

Rosa centifolia and Rosa gruss an teplitz distillation waste biomass was immobilized using sodium alginate for Pb(II) uptake from aqueous solutions under varied experimental conditions. The maximum Pb(II) adsorption occurred at pH 5. Immobilized rose waste biomasses were modified physically and chemically to enhance Pb(II) removal. The Langmuir sorption isotherm and pseudo-second-order kinetic models fitted well to the adsorption data of Pb(II) by immobilized Rosa centifolia and Rosa gruss an teplitz. The adsorbed metal is recovered by treating immobilized biomass with different chemical reagents (H(2)SO(4), HCl and H(3)PO(4)) and maximum Pb(II) recovered when treated with sulphuric acid (95.67%). The presence of cometals Na, Ca(II), Al(III), Cr(III), Cr(VI), and Cu(II), reduced Pb(II) adsorption on Rosa centifolia and Rosa gruss an teplitz waste biomass. It can be concluded from the results of the present study that rose waste can be effectively used for the uptake of Pb(II) from aqueous streams.

Fourier Transform Infrared Spectroscopic characterization and optimization of Pb(II) biosorption by fish (Labeo rohita) scales.

The present study reports the use of locally available fish (Labeo rohita) scales for Pb(II) removal from aqueous solutions under different experimental conditions. Maximum Pb(II) adsorption (196.8 mg g(-1)) occurred at pH 3.5. Pb(II) sorption was found to be pH, dose, initial metal concentration, contact time and shaking speed dependent while particle size and temperature independent. Experimental data of Pb(II) biosorption onto fish scales fitted well to Freundlich isotherm model in comparison to the model of Langmuir. The fast adsorption process in first 30 min followed by subsequent slow adsorption rate was suitably described by pseudo-second order model. In addition, this study was designed to evaluate the effect of physical and chemical pretreatments on surface properties of fish scales by the application of Fourier Transform Infrared (FTIR) Spectroscopic analysis. Physical pretreatments resulted in partial degradation of some functional groups. Alkaline pretreatments of fish scales did not have any significant influence on the nature of functional groups responsible for Pb(II) uptake, while acidic pretreatments resulted in degeneration of the most of functional groups on biosorbent cell wall. FTIR analysis confirmed the involvement of amino, carboxylic, phosphate and carbonyl groups in Pb(II) biosorption by fish scales.

Spectrophotometric determination of tranexamic acid in pharmaceutical bulk and dosage forms.

In this study, a simple, fast, accurate and sensitive spectrophotometric method has been developed for the determination of tranexamic acid in bulk and pharmaceutical preparations. The method is based on the reaction of ninhydrin with the primary amino group of tranexamic acid in the basic medium at pH 8.0. The reaction produces a bluish-purple color which absorbs maximally at 565 nm. Beer's law was obeyed in the range of 3-40 microg ml(-1) with molar absorptivity of 5.093 x 10(3) L mol(-1) cm(-1). The effects of various factors such as temperature, heating time, concentration of reagent, color stability and interferences were investigated to optimize the procedure. The results have been validated analytically and statistically. The proposed method has been applied for the determination of tranexamic acid in bulk and pharmaceutical preparations with good results.