A simple and rapid HPTLC analytical method has been developed and validated for the determination of Etanercept and Filgrastim in pure form and in marketed formulation. Both the drugs were chromatographed on silica ge...A simple and rapid HPTLC analytical method has been developed and validated for the determination of Etanercept and Filgrastim in pure form and in marketed formulation. Both the drugs were chromatographed on silica gel 60 F254s HPTLC plates, as stationary phase. The mobile phase optimized for Filgrastim and Etanercept was Water: n-butanol (7.5:2.5 v/v) and Isopropyl alcohol: water (6.5:4.5 v/v), respectively. The chromatogram obtained was scanned at 225 nm and 222 nm for filgrastim and etanercept which resulted in a retention factor of 0.45 ± 0.07 and 0.32 ± 0.03, respectively. The method was validated for parameters like linearity, accuracy, precision, specificity and robustness. Recovery studies were performed at three concentration levels, to demonstrate suitability, accuracy and precision of proposed method. Statistical analysis proved that the proposed method is accurate and reproducible with linearity in the range of 500 to 3000 ng/band for filgrastim and 200 to 1200 ng/band for etanercept. The limit of detection and limit of quantification for filgrastim was found to be 63.418 ng/band and 192.177 ng/band. For etanercept, LOD and LOQ were found to be 33.381 ng/band and 101.153 ng/band, respectively. The proposed method can be employed for the routine analysis of selected biosimilars.展开更多
A general and convenient practical approach for the synthesis of polyhydroquinoline derivatives has been achieved via one-pot four-component Hantzsch condensation of aromatic aldehydes, dimedone, ethyl acetoacetate an...A general and convenient practical approach for the synthesis of polyhydroquinoline derivatives has been achieved via one-pot four-component Hantzsch condensation of aromatic aldehydes, dimedone, ethyl acetoacetate and ammonium acetate in the presence of a catalytic amount of cerium(IV) ammonium nitrate (CAN), in ethanol solvent at ambient temperature. Simple work-up, mild reaction conditions, inexpensive and non-toxic catalyst, and excellent product yields are the advantageous features of this method.展开更多
Suzuki-Miyaura coupling reaction of N-protected 4-iodopheyl alanine isoxazoles with arylboronic acids,catalyzed by palladium,efficiently produce benzyl-N-(4-bipheyl)-2-(3-methyl-5(E)-2-aryl-1-ethenyl-4-isoxazolyl...Suzuki-Miyaura coupling reaction of N-protected 4-iodopheyl alanine isoxazoles with arylboronic acids,catalyzed by palladium,efficiently produce benzyl-N-(4-bipheyl)-2-(3-methyl-5(E)-2-aryl-1-ethenyl-4-isoxazolyl)-amino-2-oxoethyl)carba- mates in good yields.This process is first of its kind to construct carbon-carbon bond formation having biaryl motif on amino acid linked isoxazole moiety.展开更多
Tissue engineering scaffolds require a controlled pore size and interconnected pore structures to support the host tissue growth. In the present study, three dimensional (3D) hybrid scaffolds of poly lactic acid (...Tissue engineering scaffolds require a controlled pore size and interconnected pore structures to support the host tissue growth. In the present study, three dimensional (3D) hybrid scaffolds of poly lactic acid (PLA) and poly glycolic acid (PGA) were fabricated using solvent casting/particulate leaching. In this case, partially fused NaCl particles were used as porogen (200-300μ) to improve the overall porosity (≥90%) and internal texture of scaffolds. Differential scanning calorimeter (DSC) analysis of these porous scaffolds revealed a gradual reduction in glass transition temperature (Tg) (from 48°C to 42.5°C) with increase in hydrophilic PGA content. The potential applications of these scaffolds as implants were further tested for their biocompatibility and biodegradability in four simulated body fluid (SBF) types in vitro. Whereas, simulated body fluid (SBF) Type1 with the optimal amount of HCO 3 ions was found to be more appropriate and sensible for testing the bioactivity of scaffolds. Among three combinations of polymer scaffolds, sample B with a ratio of 75:25 of PLA: PGA showed greater stability in body fluids (pH 7.2) with an optimum degradation rate (9% to 12% approx). X-ray diffractogram also confirmed a thin layer of hydroxyapatite deposition over sample B with all SBF types in vitro.展开更多
A three component one-pot protocol was investigated for the synthesis of methylene bis isoxazolo[4,5-b]-pyridine-N-oxides from commercially available materials.
A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity agains...A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity against Gram-positive bacteria viz.Bacillus subtilis(ATCC 6633),Staphylococcus aureus(ATCC 6538p) and Micrococcus luteus(IFC 12708),and Gram-negative bacteria viz. Proteus vulgaris(ATCC 3851).Salmonella typhimurium(ATCC 14028) and Escherichia coli(ATCC 25922).Among the screened compounds,5d,5e,5f,5g,and 5j exhibited potent inhibitory activity compared to standard drug,and emerged as potential molecules for further development.展开更多
In this paper, we have investigated second Hankel determinants and FeketeSzeg? inequalities for some subclasses of Bi-univalent functions with respect to symmetric and Conjugate points which are subordinate to a shell...In this paper, we have investigated second Hankel determinants and FeketeSzeg? inequalities for some subclasses of Bi-univalent functions with respect to symmetric and Conjugate points which are subordinate to a shell shaped region in the open unit disc ?.展开更多
An efficient solid phase route for the synthesis of amide derivatives by the reaction of carboxylic acids with urea in the presence of catalytic amount of zirconyl chloride under microwave irradiation conditions was d...An efficient solid phase route for the synthesis of amide derivatives by the reaction of carboxylic acids with urea in the presence of catalytic amount of zirconyl chloride under microwave irradiation conditions was described. In this way, a range of interesting amide derivatives was obtained in good to excellent yields. The catalyst was recycled with fresh reactants and it gave almost similar results without significant loss of activity up to the third run.展开更多
A simple chiral HPLC method was developed and validated for quantification of S(-)-Carvedilol in Active Pharmaceutical Ingredient (API) and marketed tablet formulation of racemic Carvedilol. Chiral resolution of enant...A simple chiral HPLC method was developed and validated for quantification of S(-)-Carvedilol in Active Pharmaceutical Ingredient (API) and marketed tablet formulation of racemic Carvedilol. Chiral resolution of enantiomers of Carvedilol was achieved on Phenomenex Lux-cellulose–4 (250 mm × 4.6 mm;5 μ particle size) chiral column by using a mobile phase, Isopropanol and n-Heptane (60:40 v/v), at a flow rate of 1.0 ml/min and by employing UV detection at 254 nm wavelength. The method was validated according to the ICH guidelines and was proved to be specific, linear, precise and accurate for the analysis of S(-)-Carvedilol.展开更多
An efficient route for the synthesis of 5-(arylpropenylidine)-2,4,6-pyrimidinetrione 3 from an appropriate α,βunsaturated aromatic aldehydes 1 and barbituric acid 2 under both non-catalytic and solvent-free microw...An efficient route for the synthesis of 5-(arylpropenylidine)-2,4,6-pyrimidinetrione 3 from an appropriate α,βunsaturated aromatic aldehydes 1 and barbituric acid 2 under both non-catalytic and solvent-free microwave irradiation conditions was described. In this way, a range of biologically important compounds 3 was obtained in good to excellent yields (86-98%) in a very short reaction time (30-80 s).展开更多
The synthesis of a new series of 3-(5-substituted benzimidazol-2-yl)-5-arylisoxazolines (6a-h) was achieved in excellent yields by the condensation of 1-(1H-benzimidazol-2-yl)-3-(substituted phenyl)prop-2-en-l...The synthesis of a new series of 3-(5-substituted benzimidazol-2-yl)-5-arylisoxazolines (6a-h) was achieved in excellent yields by the condensation of 1-(1H-benzimidazol-2-yl)-3-(substituted phenyl)prop-2-en-l-ones (5a-h) with hydroxylamine at room temperature. These 1-(1H-benzimidazol-2-yl)-3-(subsfituted phenyl)prop-2-en-l-ones (Sa-h) were obtained by the condensation of 2-acetyl benzimidazoles (4a-d) with different aromatic aldehydes, which in turn were obtained by the oxidation of 2-(α- hydroxy)ethyl benzimidazoles (3a-d) prepared by the reaction of o-phenylenediamines (lad) with ot-hydroxy propiohic acid 2. The synthesized compounds were characterized by their IR, ^1H NMR and MS analyses. These compounds were screened for their antibacterial and antifungal activity by standard methods and found some of them active.展开更多
The gamma quanta attenuation studies have been carried out to determine mass attenuation coefficients of 7041, 7075 and 7095 wrought aluminum alloys. The temperature dependence of linear attenuation coefficient, densi...The gamma quanta attenuation studies have been carried out to determine mass attenuation coefficients of 7041, 7075 and 7095 wrought aluminum alloys. The temperature dependence of linear attenuation coefficient, density and thermal expansion of these wrought aluminum alloys in the temperature range 300 K - 850 K have been reported. The measurements were done by using a gamma ray densitometer designed and fabricated in our laboratory. The data on variation of density and linear thermal expansion with temperature have been represented by linear equations. Volume thermal expansion coefficients have been reported.展开更多
The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar...The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The <i>λ</i><sub>max</sub> of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.展开更多
A simple and sensitive fluorescence detection of domperidone by ultra fast liquid chromatographic method was developed and validated in human serum. For the evaluation of new drug delivery systems, conducting of pharm...A simple and sensitive fluorescence detection of domperidone by ultra fast liquid chromatographic method was developed and validated in human serum. For the evaluation of new drug delivery systems, conducting of pharmacokinetic studies in human volunteers is essential for approval to marketing after preclinical evaluation in animal models. The present method consists of protein precipitation, extraction of analytes from human serum into dichloromethane and separation using reversed-phase C<sub>18</sub> column. Propranolol hydrochloride was used as an internal standard and the eluent was monitored by fluorescence detector at excitation 282 and emission 328 nm. The mobile phase used was 62:38 ratio of 10 mM phosphate buffer pH adjusted to 3.1 with OPA and methanol at a flow rate of 1 mL·min<sup>-1</sup>. The method was evaluated for assay, LLOD, LLOQ, recovery and stability studies. The retention times for domperidone and propranolol hydrochloride were found to be 6.36 and 7.94 minutes respectively. The intraday and inter-day coefficient of variation and percent error values of assay method were less than 5%;mean recovery was more than 96% for each analyte and the method was found to be precise, accurate and specific during study. The method was successfully applied for pharmacokinetic study of immediate and controlled release bioadhesive hot melt extruded buccal patches of domperidone after buccal administration to healthy human volunteers. The C<sub>max</sub>, T<sub>max</sub>, and AUC<sub>0–24 </sub>of domperidone from immediate and controlled release buccal patches were found to be 129.7 ng·mL<sup>-1</sup>, 1.5 h, 455.1 ng·h·mL<sup>-1</sup> and 145.7 ng·mL<sup>-1</sup>, 5.25 h, 911.0 ng·h·mL<sup>-1</sup> respectively. A simple, sensitive and reliable method for the fluorescence determination of domperidone in human serum by UFLC method was developed and validated.展开更多
The present study reports a protocol for germination of Strychnos potatorum (ver. Tel. Chilla) using zygotic embryo culture as an embryo rescue method. A 100% germination rate was obtained by culturing the embryos o...The present study reports a protocol for germination of Strychnos potatorum (ver. Tel. Chilla) using zygotic embryo culture as an embryo rescue method. A 100% germination rate was obtained by culturing the embryos on full-strength Murashige and Skoog's medium (MS) containing 20 g/L sucrose in comparison to McCown and Lloyd's Woody Plant Medium (WPM). Germination rates decreased when the sucrose concentration was lower or higher than 20 g·L-1 . WPM/MS medium containing glucose at levels 30, 20, 15 g·L-1 showed a smaller percentage of germination and at quarter strength, WPM/MS medium with glucose did not respond. Multiple shoot formation was found at 1.0 2.0 mg/L BAP; 3.0 mg/L Kn; 2.0 mg/L TDZ on MS medium with 20 g·L-1 sucrose. Germination rates improved when the embryos were placed upright (vertically) in the medium. The in vitro germinated seedlings were acclimatized in a walk-in-chamber and maintained in the green house with the survival rate of 65% 75%. These plants were transferred to the field and were found to be phenotypically normal, healthy and similar to donor plants. This protocol will be useful to overcome seed dormancy and for rapid multiplication and conservation of S. potatorum using zygotic embryo culture.展开更多
An efficient synthesis of 3,4-dihydropyrimidine 2 (1H)-ones and thiones (3,4-DHPMs) core was prepared by one-pot threecomponent Biginelli condensation and which was catalyzed by trifluoromethane sulfonic acid. The...An efficient synthesis of 3,4-dihydropyrimidine 2 (1H)-ones and thiones (3,4-DHPMs) core was prepared by one-pot threecomponent Biginelli condensation and which was catalyzed by trifluoromethane sulfonic acid. The classical BigneUi reaction has been extended by the use of N-substituted benzoxazolyl semicarbazides and thiosemicarbazides and this method has the advantage of excellent yields and short reaction times. ?2009 M. Saranga Pard. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.展开更多
Among the microorganisms employed in the study,Aspergillus niger(GUFCC5443),Escherichia coli(ATCC9637),Streptomyces halstedii(CKM-2),Pseudomonas putida(NCIB9494),Cunninghamella elegans(NCIM689)and Sphingomonas paucimo...Among the microorganisms employed in the study,Aspergillus niger(GUFCC5443),Escherichia coli(ATCC9637),Streptomyces halstedii(CKM-2),Pseudomonas putida(NCIB9494),Cunninghamella elegans(NCIM689)and Sphingomonas paucimobilis(NCTC11030)were capable for the enantioselective conversion of racemic Carvedilol.Immobilization technique enhanced the enantioselectivity of microorganisms and thus increased the enantiomeric purity of the drug.Excellent enantiomeric ratios(E)were found in reactions catalyzed by immobilized A.niger and E.coli with values 174.44 and 104.26,respectively.Triacylglycerol lipase from Aspergillus niger was also employed in this study as a biocatalyst which resulted in the product with 83.35%enantiomeric excess(ee)and E of 11.34 while the enzyme on immobilization has yielded 99.08%ee and 216.39 E.The conversion yield(C%)of the drug by free-enzyme was 57.42%,which was enhanced by immobilization to 90.51%.Hence,our results suggest that immobilized triacylglycerol lipase from A.niger(Lipase AP6)could be an efficient biocatalyst for the enantioselective resolution of racemic Carvedilol to(S)-(-)-Carvedilol with high enantiomeric purity followed by immobilized cultures of A.niger and E.coli.展开更多
The synthesis of a new series of six-membered N,N′-diarylsubstituted methylene-bis-dihydro-2H-1,3-benzoxazines (5a-e) was achieved in excellent yields by Mannich-type condensation of N,N′-diarylsubstituted methyle...The synthesis of a new series of six-membered N,N′-diarylsubstituted methylene-bis-dihydro-2H-1,3-benzoxazines (5a-e) was achieved in excellent yields by Mannich-type condensation of N,N′-diarylsubstituted methylene-bis-o-hydroxybenzyl amines (4a- e) with formaldehyde in chloroform at reflux. These amines (4a-e) were obtained by the reduction of N, Nr-diarylsubstituted methylene-bis-o-hydroxybenzyl imines (3a-e) with NaBH4, which inturn were obtained by the condensation of methylene-bissalicylaldehyde (2) with various substituted arylamines.展开更多
Synthesis of novel 3-aryl-5-(3,5-dimethylisoxazol-4-yl)-2,3,5,6-tetrahydrobenzo[g][1,3,5],oxadiazocine-4-thiones 5 has been accomplished from 3,5-dimethylisoxazol-4-amine 1 by condensation with salicylaldehydes, fol...Synthesis of novel 3-aryl-5-(3,5-dimethylisoxazol-4-yl)-2,3,5,6-tetrahydrobenzo[g][1,3,5],oxadiazocine-4-thiones 5 has been accomplished from 3,5-dimethylisoxazol-4-amine 1 by condensation with salicylaldehydes, followed by reduction, treatment with aryl isothiocyanates and subsequent smooth ring closure via acetal formation in the presence of formaldehyde.展开更多
Six triphenylmethane dyes viz., bromophenol blue, basic fuchsin, methyl violet, methyl green, ethyl violet and malachite green were studied for their decolorization by Fomitopsis feei. Among, basic fuchsin (98%) was m...Six triphenylmethane dyes viz., bromophenol blue, basic fuchsin, methyl violet, methyl green, ethyl violet and malachite green were studied for their decolorization by Fomitopsis feei. Among, basic fuchsin (98%) was maximum decolorized followed by bromophenol blue (96.8%). However, the rate of bromophenol blue decolorization was very fast. There was no correlation between the lignolytic activity and dye decolurization of the dyes. The highest laccase and lignin peroxidase activities were observed in basic fuchsin (46 U/mL) and methyl green (44 U/mL) respectively after 21 days of incubation, which were poor dye degraders. The triphenylmethane reductase enzyme was the responsible enzyme for the decolorization of these triphenyl methane dyes. The treatment by using fungal organisms was considered to be the cost-effective and ecofriendly method of decolourization of effluents discharged from the dye industries.展开更多
文摘A simple and rapid HPTLC analytical method has been developed and validated for the determination of Etanercept and Filgrastim in pure form and in marketed formulation. Both the drugs were chromatographed on silica gel 60 F254s HPTLC plates, as stationary phase. The mobile phase optimized for Filgrastim and Etanercept was Water: n-butanol (7.5:2.5 v/v) and Isopropyl alcohol: water (6.5:4.5 v/v), respectively. The chromatogram obtained was scanned at 225 nm and 222 nm for filgrastim and etanercept which resulted in a retention factor of 0.45 ± 0.07 and 0.32 ± 0.03, respectively. The method was validated for parameters like linearity, accuracy, precision, specificity and robustness. Recovery studies were performed at three concentration levels, to demonstrate suitability, accuracy and precision of proposed method. Statistical analysis proved that the proposed method is accurate and reproducible with linearity in the range of 500 to 3000 ng/band for filgrastim and 200 to 1200 ng/band for etanercept. The limit of detection and limit of quantification for filgrastim was found to be 63.418 ng/band and 192.177 ng/band. For etanercept, LOD and LOQ were found to be 33.381 ng/band and 101.153 ng/band, respectively. The proposed method can be employed for the routine analysis of selected biosimilars.
文摘A general and convenient practical approach for the synthesis of polyhydroquinoline derivatives has been achieved via one-pot four-component Hantzsch condensation of aromatic aldehydes, dimedone, ethyl acetoacetate and ammonium acetate in the presence of a catalytic amount of cerium(IV) ammonium nitrate (CAN), in ethanol solvent at ambient temperature. Simple work-up, mild reaction conditions, inexpensive and non-toxic catalyst, and excellent product yields are the advantageous features of this method.
文摘Suzuki-Miyaura coupling reaction of N-protected 4-iodopheyl alanine isoxazoles with arylboronic acids,catalyzed by palladium,efficiently produce benzyl-N-(4-bipheyl)-2-(3-methyl-5(E)-2-aryl-1-ethenyl-4-isoxazolyl)-amino-2-oxoethyl)carba- mates in good yields.This process is first of its kind to construct carbon-carbon bond formation having biaryl motif on amino acid linked isoxazole moiety.
文摘Tissue engineering scaffolds require a controlled pore size and interconnected pore structures to support the host tissue growth. In the present study, three dimensional (3D) hybrid scaffolds of poly lactic acid (PLA) and poly glycolic acid (PGA) were fabricated using solvent casting/particulate leaching. In this case, partially fused NaCl particles were used as porogen (200-300μ) to improve the overall porosity (≥90%) and internal texture of scaffolds. Differential scanning calorimeter (DSC) analysis of these porous scaffolds revealed a gradual reduction in glass transition temperature (Tg) (from 48°C to 42.5°C) with increase in hydrophilic PGA content. The potential applications of these scaffolds as implants were further tested for their biocompatibility and biodegradability in four simulated body fluid (SBF) types in vitro. Whereas, simulated body fluid (SBF) Type1 with the optimal amount of HCO 3 ions was found to be more appropriate and sensible for testing the bioactivity of scaffolds. Among three combinations of polymer scaffolds, sample B with a ratio of 75:25 of PLA: PGA showed greater stability in body fluids (pH 7.2) with an optimum degradation rate (9% to 12% approx). X-ray diffractogram also confirmed a thin layer of hydroxyapatite deposition over sample B with all SBF types in vitro.
文摘A three component one-pot protocol was investigated for the synthesis of methylene bis isoxazolo[4,5-b]-pyridine-N-oxides from commercially available materials.
文摘A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity against Gram-positive bacteria viz.Bacillus subtilis(ATCC 6633),Staphylococcus aureus(ATCC 6538p) and Micrococcus luteus(IFC 12708),and Gram-negative bacteria viz. Proteus vulgaris(ATCC 3851).Salmonella typhimurium(ATCC 14028) and Escherichia coli(ATCC 25922).Among the screened compounds,5d,5e,5f,5g,and 5j exhibited potent inhibitory activity compared to standard drug,and emerged as potential molecules for further development.
文摘In this paper, we have investigated second Hankel determinants and FeketeSzeg? inequalities for some subclasses of Bi-univalent functions with respect to symmetric and Conjugate points which are subordinate to a shell shaped region in the open unit disc ?.
文摘An efficient solid phase route for the synthesis of amide derivatives by the reaction of carboxylic acids with urea in the presence of catalytic amount of zirconyl chloride under microwave irradiation conditions was described. In this way, a range of interesting amide derivatives was obtained in good to excellent yields. The catalyst was recycled with fresh reactants and it gave almost similar results without significant loss of activity up to the third run.
文摘A simple chiral HPLC method was developed and validated for quantification of S(-)-Carvedilol in Active Pharmaceutical Ingredient (API) and marketed tablet formulation of racemic Carvedilol. Chiral resolution of enantiomers of Carvedilol was achieved on Phenomenex Lux-cellulose–4 (250 mm × 4.6 mm;5 μ particle size) chiral column by using a mobile phase, Isopropanol and n-Heptane (60:40 v/v), at a flow rate of 1.0 ml/min and by employing UV detection at 254 nm wavelength. The method was validated according to the ICH guidelines and was proved to be specific, linear, precise and accurate for the analysis of S(-)-Carvedilol.
文摘An efficient route for the synthesis of 5-(arylpropenylidine)-2,4,6-pyrimidinetrione 3 from an appropriate α,βunsaturated aromatic aldehydes 1 and barbituric acid 2 under both non-catalytic and solvent-free microwave irradiation conditions was described. In this way, a range of biologically important compounds 3 was obtained in good to excellent yields (86-98%) in a very short reaction time (30-80 s).
文摘The synthesis of a new series of 3-(5-substituted benzimidazol-2-yl)-5-arylisoxazolines (6a-h) was achieved in excellent yields by the condensation of 1-(1H-benzimidazol-2-yl)-3-(substituted phenyl)prop-2-en-l-ones (5a-h) with hydroxylamine at room temperature. These 1-(1H-benzimidazol-2-yl)-3-(subsfituted phenyl)prop-2-en-l-ones (Sa-h) were obtained by the condensation of 2-acetyl benzimidazoles (4a-d) with different aromatic aldehydes, which in turn were obtained by the oxidation of 2-(α- hydroxy)ethyl benzimidazoles (3a-d) prepared by the reaction of o-phenylenediamines (lad) with ot-hydroxy propiohic acid 2. The synthesized compounds were characterized by their IR, ^1H NMR and MS analyses. These compounds were screened for their antibacterial and antifungal activity by standard methods and found some of them active.
文摘The gamma quanta attenuation studies have been carried out to determine mass attenuation coefficients of 7041, 7075 and 7095 wrought aluminum alloys. The temperature dependence of linear attenuation coefficient, density and thermal expansion of these wrought aluminum alloys in the temperature range 300 K - 850 K have been reported. The measurements were done by using a gamma ray densitometer designed and fabricated in our laboratory. The data on variation of density and linear thermal expansion with temperature have been represented by linear equations. Volume thermal expansion coefficients have been reported.
文摘The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The <i>λ</i><sub>max</sub> of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.
文摘A simple and sensitive fluorescence detection of domperidone by ultra fast liquid chromatographic method was developed and validated in human serum. For the evaluation of new drug delivery systems, conducting of pharmacokinetic studies in human volunteers is essential for approval to marketing after preclinical evaluation in animal models. The present method consists of protein precipitation, extraction of analytes from human serum into dichloromethane and separation using reversed-phase C<sub>18</sub> column. Propranolol hydrochloride was used as an internal standard and the eluent was monitored by fluorescence detector at excitation 282 and emission 328 nm. The mobile phase used was 62:38 ratio of 10 mM phosphate buffer pH adjusted to 3.1 with OPA and methanol at a flow rate of 1 mL·min<sup>-1</sup>. The method was evaluated for assay, LLOD, LLOQ, recovery and stability studies. The retention times for domperidone and propranolol hydrochloride were found to be 6.36 and 7.94 minutes respectively. The intraday and inter-day coefficient of variation and percent error values of assay method were less than 5%;mean recovery was more than 96% for each analyte and the method was found to be precise, accurate and specific during study. The method was successfully applied for pharmacokinetic study of immediate and controlled release bioadhesive hot melt extruded buccal patches of domperidone after buccal administration to healthy human volunteers. The C<sub>max</sub>, T<sub>max</sub>, and AUC<sub>0–24 </sub>of domperidone from immediate and controlled release buccal patches were found to be 129.7 ng·mL<sup>-1</sup>, 1.5 h, 455.1 ng·h·mL<sup>-1</sup> and 145.7 ng·mL<sup>-1</sup>, 5.25 h, 911.0 ng·h·mL<sup>-1</sup> respectively. A simple, sensitive and reliable method for the fluorescence determination of domperidone in human serum by UFLC method was developed and validated.
基金supported by UGC,for financial assistance as Project Fellow under UGC-SAP-DRS-I programme(Ref. No. 558/UGC/KU/2010)
文摘The present study reports a protocol for germination of Strychnos potatorum (ver. Tel. Chilla) using zygotic embryo culture as an embryo rescue method. A 100% germination rate was obtained by culturing the embryos on full-strength Murashige and Skoog's medium (MS) containing 20 g/L sucrose in comparison to McCown and Lloyd's Woody Plant Medium (WPM). Germination rates decreased when the sucrose concentration was lower or higher than 20 g·L-1 . WPM/MS medium containing glucose at levels 30, 20, 15 g·L-1 showed a smaller percentage of germination and at quarter strength, WPM/MS medium with glucose did not respond. Multiple shoot formation was found at 1.0 2.0 mg/L BAP; 3.0 mg/L Kn; 2.0 mg/L TDZ on MS medium with 20 g·L-1 sucrose. Germination rates improved when the embryos were placed upright (vertically) in the medium. The in vitro germinated seedlings were acclimatized in a walk-in-chamber and maintained in the green house with the survival rate of 65% 75%. These plants were transferred to the field and were found to be phenotypically normal, healthy and similar to donor plants. This protocol will be useful to overcome seed dormancy and for rapid multiplication and conservation of S. potatorum using zygotic embryo culture.
文摘An efficient synthesis of 3,4-dihydropyrimidine 2 (1H)-ones and thiones (3,4-DHPMs) core was prepared by one-pot threecomponent Biginelli condensation and which was catalyzed by trifluoromethane sulfonic acid. The classical BigneUi reaction has been extended by the use of N-substituted benzoxazolyl semicarbazides and thiosemicarbazides and this method has the advantage of excellent yields and short reaction times. ?2009 M. Saranga Pard. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.
基金Authors are thankful for the financial assistance(SR/SO/HS/0087/2010)given by Science and Engineering Research Board,DST,New Delhi,India.Authors are also thankful to Symed labs Ltd.,Medak,India,for the kind gift of racemic Carvedilol.
文摘Among the microorganisms employed in the study,Aspergillus niger(GUFCC5443),Escherichia coli(ATCC9637),Streptomyces halstedii(CKM-2),Pseudomonas putida(NCIB9494),Cunninghamella elegans(NCIM689)and Sphingomonas paucimobilis(NCTC11030)were capable for the enantioselective conversion of racemic Carvedilol.Immobilization technique enhanced the enantioselectivity of microorganisms and thus increased the enantiomeric purity of the drug.Excellent enantiomeric ratios(E)were found in reactions catalyzed by immobilized A.niger and E.coli with values 174.44 and 104.26,respectively.Triacylglycerol lipase from Aspergillus niger was also employed in this study as a biocatalyst which resulted in the product with 83.35%enantiomeric excess(ee)and E of 11.34 while the enzyme on immobilization has yielded 99.08%ee and 216.39 E.The conversion yield(C%)of the drug by free-enzyme was 57.42%,which was enhanced by immobilization to 90.51%.Hence,our results suggest that immobilized triacylglycerol lipase from A.niger(Lipase AP6)could be an efficient biocatalyst for the enantioselective resolution of racemic Carvedilol to(S)-(-)-Carvedilol with high enantiomeric purity followed by immobilized cultures of A.niger and E.coli.
文摘The synthesis of a new series of six-membered N,N′-diarylsubstituted methylene-bis-dihydro-2H-1,3-benzoxazines (5a-e) was achieved in excellent yields by Mannich-type condensation of N,N′-diarylsubstituted methylene-bis-o-hydroxybenzyl amines (4a- e) with formaldehyde in chloroform at reflux. These amines (4a-e) were obtained by the reduction of N, Nr-diarylsubstituted methylene-bis-o-hydroxybenzyl imines (3a-e) with NaBH4, which inturn were obtained by the condensation of methylene-bissalicylaldehyde (2) with various substituted arylamines.
文摘Synthesis of novel 3-aryl-5-(3,5-dimethylisoxazol-4-yl)-2,3,5,6-tetrahydrobenzo[g][1,3,5],oxadiazocine-4-thiones 5 has been accomplished from 3,5-dimethylisoxazol-4-amine 1 by condensation with salicylaldehydes, followed by reduction, treatment with aryl isothiocyanates and subsequent smooth ring closure via acetal formation in the presence of formaldehyde.
文摘Six triphenylmethane dyes viz., bromophenol blue, basic fuchsin, methyl violet, methyl green, ethyl violet and malachite green were studied for their decolorization by Fomitopsis feei. Among, basic fuchsin (98%) was maximum decolorized followed by bromophenol blue (96.8%). However, the rate of bromophenol blue decolorization was very fast. There was no correlation between the lignolytic activity and dye decolurization of the dyes. The highest laccase and lignin peroxidase activities were observed in basic fuchsin (46 U/mL) and methyl green (44 U/mL) respectively after 21 days of incubation, which were poor dye degraders. The triphenylmethane reductase enzyme was the responsible enzyme for the decolorization of these triphenyl methane dyes. The treatment by using fungal organisms was considered to be the cost-effective and ecofriendly method of decolourization of effluents discharged from the dye industries.