The problems of synthetic pigment causing toxicity and carcinogenicity in the human body decrease its use. Therefore, interest in natural pigment production is increasing. Therefore, the marine environment has recently become an attractive research subject for many investigations, because of its rich biodiversity. Attempt has been initiated to isolate Micrococcus luteus from marina beach water. The sea water sample isolated was allowed to grow in a Zobell marine agar medium and incubated at 37 °C for one week. The isolated strain from marine source was confirmed by 16S rRNA sequencing. The GC content was found to be 58.6%. Phylogenetic tree analysis was performed to know the sequences that are closely related. The strain was assessed for pigment production in Zobell marine broth and incubated at 37 °C for two days. The swab sticks collected from hospital were streaked directly on the labelled agar plates such as eosin methylene blue, MacConkey, nutrient, blood, mannitol salt agar and incubated at 37 °C for 24 h and characterized. The antibacterial activity of crude pigment was tested against wound isolates. The individual yellow colour colonies obtained was sequenced, submitted to gene bank under the accession number KF532949. Phylogenetic analysis revealed, that the identified strain M. luteus is closely related to various Micrococcus sp. The crude pigment showed promising results against Staphylococcus sp., Klebsiella sp., Pseudomonas sp. isolated from wound. From this result, we can conclude that the isolated strain M. luteus is able to act against both gram positive and gram negative bacteria.
Background/aimIn the present study, a series of novel phthalimide derivatives synthesized because of its potent antimicrobial and antimycobacterial activity.MethodStructurally modified phthalimide derivatives were prepared through condensation of substituted phthalic anhydride with corresponding acetazolamide, cycloserine and isoniazid with variable yields. Synthesized Compounds (6a–d), (7a–d) and (8a–d) analyzed for their structures, in vitro antimicrobial and antimycobacterial activity.ResultAmong the synthesized compounds, compound 6b, 7b and 8b was found to be the most potent against Gram-positive bacteria Bacillus subtilis, Gram-negative bacteria Escherichia coli, Mycobacterium tuberculosis CIP and M. tuberculosis H37Rv.ConclusionA series of novel phthalimide derivatives of biological interest were synthesized and analyzed, suggests that it an interesting compound compared to the current therapeutic agents and are considered to investigate further for the same.
Background/ObjectiveA direct, accurate, precise, reproducible and cost-time efficient approach for calibration of HPLC using mass spectrometer as detector has been described which simulates the routine analysis in bioanalytical laboratories.MethodsInjector position check and injection volume repeatability test for the calibration of autosampler; and pump flow rate accuracy test for the calibration of pumps were illustrated using direct weighing method. Carryover test, pump repeatability test, linearity and precision were carried out for holistic (overall system) calibration of the instrument using a sensitive high throughput LC–MS/MS pre-validated method.Results/ConclusionThe results of calibration experiments for individual modules suggested that pumps are yielding accurate flow rate, autosampler is aspirating the correct injection volume irrespective to position or volume, and column oven and autosampler chambers are maintaining steady temperatures. Holistic calibration verified the accuracy, precision, repeatability and reproducibility of the instrument with insignificant carryover.
Aim Graphene oxide/polypyrrole nanocomposites (PNCs) with enhanced electrocapacitive performance were prepared through a cationic surfactant assisted dilute solution polymerization of pyrrole in presence of GO at various concentrations (%, w/w) ranging 10.0–40.0 and ferric chloride as oxidant. Methods PNCs has been characterized through Fourier transformed infrared spectra, X-ray diffraction, scanning electron microscopy and simultaneous thermogravimetric-differential scanning caloriemetry. Electrochemical capacitance (Cs, F/g) of electrodes fabricated from PNCs over 316 stainless steel in presence of sulphonated polysulphone as binder has been investigated in KOH solution (1.0 M) with reference to Ag/AgCl at scan rate (V/s) ranging 0.2–0.001. Results PNCs with 20.0%, w/w of GO have shown highest Cs of 1073.64 as compared to 92.33 for pure PPy at a scan rate of 0.001 V/s. PNCs rendered a low electrocapacitive decrease during the first 500 cycles at scan rate of 0.1 V/s indicating their appreciable electrochemical performance for fabrication of supercapacitor electrodes.
Photodegradation process and mechanism is a relative new and eco-friendly process to recycle and reuse of water. Some investigation concerned with effort to increase photocatalyst activity by immobilizing semiconductor oxide such as ZnO in clay as solid support. It was related to that photodegradation was directed by adsorption mechanism. However sometimes the activity of a photocatalyst is not linearly correlated with adsorption mechanism. In this research evaluation on photoactivity of ZnO-hectorite (ZnO/CTMA/Hectorite) and TiO2-montmorillonite based material using statistical approximation compared to the linear model is studied. The model is evaluated for photodegradation of phenol solution. Some beneficial results of the probit model are (i) the guarantee of activity prediction value in the range of 0–100% (ii) interaction of adsorption and photodegradation mechanism is well described.
AimThe extreme efforts have been developed to design novel compounds to strains of resistant micro-organisms. On-going search for novel and amazing drug delivery systems is primarily impact of the well-established fact that the convectional dosages are not sufficiently effective in conveying the drug compounds to its site of action and this has required the need to search for more efficient drugs. The metal complexes of Co (II), Ni (II) and Cu (II) with a tridentate ligand 2, 5-diamino-1, 3, 4-thiadiazole has been prepared by cyclisation of bithiourea in a 3% hydrogen peroxide medium. 2, 5-diamino-1, 3, 4-thiadiazole acts as neutral tridentate ligand and coordinates through the sulphur atom and nitrogen of the amines. The complexes are non-electrolyte in DMF. The complexes exhibited octahedral geometry. The antimicrobial activities of ligand and its complexes were screened using sensitivity test, minimum inhibition concentration and minimum bacterial concentration method. Metal chelates showed greater antimicrobial activities as compared to the control and the ligand. The metal chelates and the ligand did not exhibited activity against Aspergillus niger and Penicillin species.MethodsElemental analyses, IR spectra, magnetic susceptibilities by using Faraday Balance, molar conductance by using Genway 4200 conductivity meter. Metal estimation by using Alpha 4 Atomic Absorption Spectrophotometer. Thin layer chromatography was carried out using TLC plate coated with silica gel.ResultsThe results of the elemental analyses are in good agreement with those calculated for the suggested formulae, 1:2 (M:L) solid chelates are isolated and found to have the general formulae [(ML2)] X2; M=Co (II), Ni (II) and Cu (II) (X=Cl). The IR spectra revealed that the ligand L is a neutral tridentate ligand. It coordinated to the metal ions via the nitrogen of the amines and sulphur atom. The molar conductance values of the Co (II), Ni (II), and Cu (II) complexes were relatively low, indicating the non-electrolytic nature of these complexes. The ligand and metal complexes show antimicrobial effect against the tested organism species except against molds of penicillin and Aspergillus. Niesseria gonorrhoea was probably the most sensitive organism to the 2, 5-Diamino-1, 3, 4-Thiadizole and its metal complexes. Metal complexes showed greater activity against some of the micro-organisms compared to the parent compounds.ConclusionIn this paper we conclude from combined results of the chemical and physical analysis that the ligand (2, 5-diamino-1, 3, 4-thiadiazole) coordinated with Cu, Co and Ni. The metal complexes possess better physical properties than the parent compound. Metal complex of 2,5-diamino-1,3,4-thiadiazole would be a better therapeutic drug for antibacterial treatment.
AimIn recent years oxidative stress was found to play the significant role in causing various diseases, including neurodegenerative disorders like, Alzheimer's. Lack of antioxidant mechanisms is the major cause for increased oxidative stress. Flavonoids and phenolic compounds from herbs are going to play efficient role in scavenging the free radicals responsible for oxidative stress. Present investigation deals with the free radical scavenging activity of Leucas species in relation to neurodegenerative disorder.MethodsEthanolic extract of selected plant was estimated for phenolic and flavonoids contents and then screened for free radical scavenging activity with various oxygen radicals. The extract was further tested invitro for acetylcholinesterase inhibitory activity along with cytotoxic activity.ResultsThe extract was found to contain 42.28 ± 8.88 RE/g of flavonoids and 38.624 ± 14.171 GAE/g of phenolic compounds along with significant free radical scavenging activity in comparison with the standard Quercetin. The extract was found to be non cytotoxic with no inhibitory activity on acetylcholinesterase.ConclusionInspite of its inability to inhibit acetylcholinesterase, the selected plant extract can be safely used for treating neurodegenerative disorders like Alzheimer's because of its effective free radical scavenging activity.
Background/AimAn endophytic fungus belongs to the genus Phomopsis was isolated from stem of Ficus pumila (Moraceae) and identified based on morphological and molecular characteristics.MethodsAntimicrobial potential was investigated by agar plug, disc diffusion and TLC bioautography agar overlay methods. Detection of polyketide synthase (PKS) genes using DOP-PCR techniques.ResultsEndophytic Phomopsis sp. identified by morphological as well as molecular techniques, which exhibited broad a spectrum antimicrobial activity against Gram positive and Gram negative human and phytopathogenic bacteria and fungi. TLC bioautography detects the production of antimicrobial metabolites.ConclusionThis preliminary study revealed that endophytic Phomopsis species are prolific producer of antimicrobial metabolites with wide range of antimicrobial activity.
AimThe aim of the present study is to synthesize the metal nanoparticles by the green chemical approaches due to their novel optical, catalytic, hydrogen storage, bio-imaging and electrochemical applications.Materials and methods1 mM of PdCl2 and Piper betle leaf broth (10:1) are used to synthesize the stable Pd0 nanoparticles.ResultsThe structural characterizations studied by UV-Vis Spectroscopy, XRD and FTIR-Spectroscopy. The morphology, particle distribution and size of the palladium nanoparticles were studied by TEM and SAED Techniques. The bioactivity demonstrated by synthesized PdNPs was lead to an excellent clinical use as anti-fungal material.
Aims Diclofenac sodium is a Nonsteroidal Anti-Inflammatory Drug (NSAID) with anti-inflammatory, antipyretic, and analgesic action as a result of the blockade of prostaglandin synthesis by inhibition of the cyclooxygenase enzyme. Analysis of the active pharmaceutical ingredient as well as finished pharmaceutical product is of vital importance to help ensure that good quality products are manufactured and supplied to the patient end users. The aim of the study was to develop a simple and rapid method to enable timely release of products. Methods The method was developed using a mobile phase prepared with environment-friendly analytical grade solvents: toluene, acetone and glacial acetic acid (10:15:0.2 v/v/v). Diclofenac sodium reference material and samples were chromatographed using pre-coated TLC silica gel 60 F254 glass plates with a saturation time of 25 minutes and a densitometer detection wavelength of 284 nm in the reflectance absorbance mode. Detection and part of analysis was done using densitometer TLC Scanner 3 operated with Wincats (version 1.4.3) planar chromatograph software. Results A Thin Layer Chromatography (TLC) method for the qualitative and quantitative analysis of diclofenac sodium tablets was developed and validated according to ICH and USP guidelines. The Rf of diclofenac sodium was at 0.60 and the method was repeatable, robust with good selectivity and specificity. Regression functions were established over the range of 250–600 ng/spot with r2 of 0.993 and 0.999 for the linear and polynomial regressions respectively. The accuracy at nominal concentration was found to be 100.2%, and the results of the assay of three brands for diclofenac sodium tablets were found to meet the USP 95–105% assay limits thus demonstrating the usefulness of the method for the assay of these products.The developed assay method for diclofenac sodium in tablets is simple, accurate, and inexpensive, with good precision and should be especially useful in resource constrained countries.
BackgroundRosuvastatin is an HMG Co-A inhibitor and Ezetimibe is an intestinal cholesterol absorption inhibitor. The combination formulation is used for the treatment of hypercholestrolemia. A simple, accurate and precise assay and rapid stability-indicating reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the simultaneous estimation of Rosuvastatin (RSV) and Ezetimibe (EZE) from their combination drug product.MethodsThe proposed method is based on the separation of the two drugs in reversed-phase mode using Water’s C18 250 × 4.6 mm, 5μ column maintained at an ambient temperature. The optimum mobile phase consisted of Acetonitrile: water: 0.02 M phosphate buffer pH 8 (40:10:50 v/v), flow rate of mobile phase was set 1.0 mL min−1 and PDA detection was performed at 230 nm. The method was validated according to ICH guidelines.ResultsIt was found to be accurate and reproducible. Linearity was obtained in the concentration range of 30–90 μg mL−1 for both RSV and EZE with correlation coefficients of 0.999 and 0.998 respectively. Mean percent recovery of triplicate samples at each level for both drugs were found in the range of 98% to 100% with RSD of less than 2.0%. Rosuvastatin, Ezetimibe and their combination drug product were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions and the stressed samples were analyzed by the proposed method. There were no interfering peaks from excipients, impurities or degradation products due to variable stress conditions and the proposed method is specific for the simultaneous estimation of RSV and EZE in the presence of their degradation products.ConclusionThe proposed method can be successfully applied in the quality control and stability samples of bulk manufacturing and pharmaceutical dosage forms.
ObjectiveTo investigate antimutagenic and antioxidant potency of the aqueous heat treated Ficus benghalensis stem bark (FBH) extract and Moringa oleifera root (MRH) extract against sodium azide in TA100 tester strains of Salmonella typhimurium and their inhibition of microsomal lipid peroxidation (LPO).MethodsMutagenicity was assayed by the standard Ames test (standard plate incorporation assay) and antioxidant potency was investigated by employing ex vivo inhibition of lipid peroxidation in liver Microsomes.ResultsBoth FBH and MRH showed strong antimutagenic effect on S. typhimurium TA100 strains against sodium azide (NaN3). IC50 values of aqueous extract of FBH and MRH extracts were 70.24 μg/ml and 99.20 μg/ml respectively. FBH extract showed maximum inhibition of microsomal lipid peroxidation responses than MRH. IC50 values of aqueous extract of FBH and MRH extracts were 80.24 μg/ml and 92 μg/ml respectively. FBH and MRH exhibited a dose dependent antioxidant activity.ConclusionThe aqueous heat-treated FBH and MRH have antimutagenic as well as antioxidant activity. Further studies are in progress to evaluate the effect of both extracts by other antioxidant and antimutagenic assays and to identify the factors responsible for these activities.
AimQuantification of macronutrient, micronutrient and toxic elements from the leaves of Celocia argentea by inductively coupled plasma-optical emission spectrometry (ICP-OES) and to report efficient, reliable, eco friendly method of digestion for better recovery of the elements.MethodsThe five digestion methods are studied included, dry ashing method with HNO3/HCl, wet digestion method with HNO3/HClO4 and HNO3/H2O2, microwave digestion with HNO3/HClO4 and HNO3/H2O2. ICP-OES operating parameter was optimized at radial and axial viewing along with the radio-frequency power, sample flush time and gas flow rate. The results of the elemental quantification were statistically analyzed using one way analysis of variance (ANOVA) by Kruskal–Wallis test.ResultsC. argentea exhibits good quantity of macronutrients like Mg, Ca S, P, K and Fe. The ashing and microwave digestion method were found to more reliable as compare to wet digestion method and hence recommended for better recovery. The element Ca, Cu and Fe gives better recovery by ash and microwave digestion method as compare to wet digestion method. Toxic elements show their concentration below permissible limit.ConclusionAll the nutrients as well as toxic elements are quantified successfully by ICP-OES technique by all methods of digestion. Dry and wet digestion methods are tedious and time consuming compare to microwave digestion method, which is greener and simpler. Kruskal–Wallis test can be employed for non-parametric methods to compare more than two population average which do not require any specific form of the distribution of the population. The C. argentea can be used as supplementary food for deficiency of minerals like Fe, Mg and Ca.
ObjectiveTo develop a simple, novel, sensitive, precise and specific RP-HPLC method for the determination of Tapentadol hydrochloride in bulk and its tablet dosage forms.MethodsThe chromatographic separation was achieved on C18 Licrosphere column (150 mm × 4.6 mm inner diameter, 5 μm particle size) as a stationary phase using Methanol: 0.1 mM Dipotassium Phosphate buffer (pH 4, adjusted with ortho phosphoric acid) as mobile phase at detection wavelength 280 nm in isocratic mode at a flow rate of 1 ml/min.ResultsThe calibration curve for Tapentadol hydrochloride was linear from 75 to 450 μg/ml. The correlation coefficient (r2) value was found to be 0.9994. Precision study showed % CV value less than 2% in all selected concentrations. The % recoveries of Tapentadol hydrochloride are in the range of 99.96–100.01%. The limit of detection and limit of quantification for Tapentadol hydrochloride were found to be 0.25 μg/ml and 0.75 μg/ml respectively.ConclusionThe developed method has good sensitivity, reproducibility and specificity for the determination of Tapentadol hydrochloride in bulk and its tablet dosage forms. This method was simple, fast, accurate, and precise. Hence this method was validated and found to be suitable for determining the purity of Tapentadol hydrochloride in bulk drugs and pharmaceutical formulations. The proposed validated method was successfully used for the quantitative analysis of commercially available dosage form.
AimButyl methacrylate is used with acrylic products in order to improve the final product according to the desired characteristics. In this work we are about to make an assignment of experimental infrared bands with the help of a theoretical quantum chemistry calculations. The exact knowledge of some bands which are not characteristics of acrylic materials will enable us to make a quick analysis with available techniques of low costs for mixtures of polymers based on acrylate and methacrylate molecules.Materials and methodsIn the experimental part, the infrared spectrum of butyl methacrylate is obtained by using an FTIR Perkin Elmer model 2000. In the computational part and as first step, the theoretical calculations are performed by the semi-empirical AM1 method for excluding similar structures of butyl methacrylate molecule by a meticulous conformational analysis. As a second step the obtained structures are optimized using DFT. The simulated frequencies are then scaled and a tentative assignment is made based on band intensities and PED percentages.ResultsThe theoretical calculations predict the existence of five conformations two of them represent the majority of experimental bands in the infrared spectrum. The two less stable structures represent better the band at 546 cm−1, while the assignment is very difficult for the band at 491 cm−1.
Context Micellar thin layer chromatography (MLC) used for separation of various heavy metal ions from various environmental samples. MLC successfully applied for semiquanitative and spectrometry identification of metal ions. Objective Utilization of MLC in separation, semiquanitative determination and Chromatospectrometric method for estimation of UO22+ on bismuth silicate layer, using Tween-80. Method Ascending development of the plates performed with aq. micellar, hydro-organic and water-organic-surfactant as mobile phase. Separation carried out on thin layer of bismuth silicate and layer developed with non-ionic surfactant Tween-80. Results and conclusions Acetone was found to be most effective additive at 10% concentration with 5% Tween-80. This method successfully applied to identification and separation of Cd2, Hg2 and Co2 from river water and industrial wastewater. Semiquantitative as well as spectrometry techniques was used for quantitative analysis of UO22+ in river water with preliminary separation from Fe3 and Cu2. Maximal recovery of 90% observed. This TLC method is rapid, with development times averaging 2–5 min.
A rapid, sensitive and specific method based on high performance liquid chromatography (HPLC) has been developed for the simultaneous determination of amitriptyline hydrochloride and Sildenafil citrate in the blood of rats. Sample preparation involved liquid–liquid extraction with n-hexane after alkalified with 0.5 M NaOH. Chromatographic separation was performed on XDB C-18 column with particle size of 5 μm (150 × 4.6 mm) with mobile phase acetonitrile and 20 mM KH2PO4 buffer, pH = 3 using flow rate 1.5 ml/min. Calibration curves were linear within the ranges of 0.25–50 and 0.1–50 μg/ml for amitriptyline hydrochloride and Sildenafil citrate, respectively. This method was successfully applied to the pharmacokinetic study in rats after oral administration of amitriptyline hydrochloride and Sildenafil citrate for 24 h.
An asymmetric synthesis of the piperidine alkaloid (−)-sedridine isolated from Sedum acre, has been accomplished starting from S-malic acid as the chiral precursor employing Maruoka Keck allylation, azide nucleophillic substitution and ring closing metathesis as the key steps.
ObjectiveTo develop an efficient method for the synthesis of Methyl-2-(N-ethyl-N-phenylamino)naphthyridine-3-carboxylates which is suitable for different naphthyridines.MethodsAll reagents used were commercial grade, 1H NMR spectra were obtained on a varian 400 MHz instrument with TMS as internal standard and chemical shifts are expressed δ ppm solvent used in DMSO-d6 & CDCl3 and LC–MS spectrum on a Waters LC–MS spectrometer operating at 70 ev. TLC is performed with E-Merch precoated silica gel plates (60F-254) with iodine as a developing agent. Acme, India silica gel, 60–120 mesh for column chromatography is used. All compounds are purified by column chromatography by using Silica gel (60–120 mesh) eluted with (50:1) dichloromethane in methanol.ConclusionsWe have developed an efficient protocol for the synthesis of Methyl-2-(N-ethyl-N-phenylamino)naphthyridine-3-carboxylates.
AimsTerpolymer (BPEDF) has been synthesized by the condensation of the monomers 2, 2′- biphenol, ethylene diamine and formaldehyde in 1:1:2 molar proportions in the presence of 2 M HCl as a catalyst.MethodsThe purity of newly synthesized resin has been tested and confirmed by the thin layer chromatography (TLC) technique. The structure of BPEDF has been elucidated on the basis of elemental analysis and various physicochemical techniques, i.e. FTIR, 1HNMR, and UV–Visible spectral studies.ResultDetailed thermal degradation study of the new terpolymer has been carried out to ascertain its thermal stability. The thermal degradation curve shows three decomposition steps (40–210 °C, 220–410 °C and 410 °C–900 °C). The thermal degradation curve was examined in order to determine their mode of decomposition, order of reaction, apparent activation energy, frequency factor, free energy change, entropy change and apparent energy change. Sharp–Wentworth and Freeman–Carroll methods have been used to calculate activation energies and thermal stability. The activation energy (25.84 KJ/mole−1) calculated by using the Sharp–Wentworth method has been found to be in good agreement with that calculated by Freeman–Carroll method (23.11 KJ/mole−1). The decomposition temperature is found to be 251 °C. The order of reaction (n) is found to be 0.95.
