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ThesisItem Open Access Efficiency of Daucus carota silver nanoparticles for removal of lead ions (Pb+2) from waste water(DEPARTEMENT OF CHEMISTRY FACULTY OF SCIENCE Sam Higginbottom University of Agriculture, Technology & Sciences Prayagraj-211007(U.P.) India, 2019) SINGH, SHWETA; Chattree, Dr. AmitThe removal of Pb from wastewater is one of the major environmental concerns these days. Concerning the environmental awareness and the economical point of view, the use of low-cost and eco-friendly adsorbent has been investigated as an ideal alternative to the current expensive method of removing heavy metals from wastewater. The main objective of the present work is to study the removal of Pb from wastewater using modified agriculture product as an adsorbent i.e silver nanoparticles synthesize by using Dacus carota. All reaction parameters were conducted in batch equilibrium mode that is adsorbate concentration 10 ppm, adsorbent dose (0.01,0.02,0.03,0.04,0.05 g) , pH (3,4,5,6,7,8,9,10) and contact time (20,40,60,80,100 min). Characterization of adsorbent was done using UV-visible spectroscopy to confirm the synthesis of nanoparticles, XRD and FTIR to determine particle crystalline nature and functional groups present on the surface,respectively. The effective solution pH, adsorbent dose and contact time on the Pb adsorption were found to be 3, 0.01g, 80 min, respectively for the adsorption studies. The percentage removal is 74% at this condition. Adsorption capacity is 37.0 mg/g. Three common models that is Langmuir Freundlich and Temkin isotherms were used to investigated the interaction of Pb and adsorbent. The adsorption is best fitted by Temkin isotherm . Monolayer adsorption capacity is 13.51 mg/g. Adsorption thermodynamic was determined which suggest adsorption process is exothermic and spontaneous. The results indicate that carrot-silver nanoparticles can be used as a low cost adsorbent, as an alternative for treatment of wastewater.ThesisItem Open Access Synthesis, Characterization and Application of Ecofriendly Polymer Polylactic acid and its Blends(DEPARTMENT OF CHEMISTRY FACULTY OF SCIENCE SAM HIGGINBOTTOM UNIVERSITY OF AGRICULTURE, TECHNOLOGY AND SCIENCES PRAYAGRAJ (ALLAHABAD)-211007, U.P., INDIA, 2018) Singh, Sanjay Kumar; Anthony, Dr. PrashantA major problem all over the world is the environmental pollution caused due to plastic wastes. Raw materials used in the polymer industries are generally based on petroleum derivatives. Due to their non-degradable nature they are a serious threat to environment. Hence, there is a need to increase an interest in the production and use of biodegradable polymers. The biodegradable polymeric materials derived from renewable resources have attracted tremendous attention in different applications. Polylactic acid (PLA) is one of the most useful biodegradable polymers. However, it is difficult to synthesize high molecular weight polylactic acid by direct polycondensation. In the present work an attempt has been made to synthesize different molecular weight polylactic acid, by varying the duration of reaction as well as different catalyst. The synthesized PLA was used to make biodegradable polymer blends with non degradable polymer such PVC and PVAc. The PVC/PLA blends were prepared with and without compatibilizer (PMMA and PE-g-MAH) by solution casting method. The miscibility of blends was characterized by DSC and SEM images. The obtained results show that without compatibilizer two different glass transition temperatures were observed and large domain size indicating immiscible nature of blend. The presence of compatibilizer enhanced the interfacial interaction between two polymers and that resulted in the miscibility of the blends. The thermal and mechanical properties of blend were investigated by thermogravimetric analysis and universal testing machine. The biodegradability of blends was studied by controlled soil burial test and was analyzed by visual observation and SEM analysis. The results indicate the biodegradability of PVC/PLA blends increases with the increase of PLA constituent. The PVAc/PLA blends were prepared by solution casting method. The characteristics of PLA/PVC blend films were analyzed for thermal properties by Thermogravimetric Analysis (TGA), morphology of blends film by scanning electron microscope (SEM). The biodegradability of blend films were studied under controlled condition of soil burial test and was analyzed by visual observations, measuring weight loss and by morphological analysis.ThesisItem Open Access GRAPHENE OXIDE SUPPORTED HETEROGENEOUS ACID CATALYSTS FOR THE ESTERIFICATION OF OLEIC ACID AND CONVERSION OF WASTE COOKING OIL TO BIODIESEL(Department of chemistry Sam Higginbottom University of Agriculture, Technology & Sciences, Allahabad 211007 (UP) I.D NO.12PHHSHD103, 2019) Reena D, Souza R; Chattree, Dr. AmitGraphene supported acid catalyst is a heterogeneous catalyst which is an eco-friendly catalyst as it is less hazardous and can be recycled. Biodiesel obtained from waste cooking oil (WCO) or animal fat is an example of a renewable source of energy. Thus, in the present study, preparation of graphene oxide GO, GO-Fe2O3, GO-SO3H, GO-Fe2O3-SO3H, GO-CoO-SO3H, GO-NiO-SO3H, GO-CuO-SO3H and GO-ZnO-SO3H for the esterification of oleic acid and conversion of WCO to biodiesel using ethanol was carried out successfully. The catalytic activities of these catalysts were evaluated in the esterification of oleic acid using ethanol. The reaction conditions for esterification reaction were temperature 900 C, time 4 h, acid to alcohol ratio 1:12, 5 wt % of catalyst in a water-cooled reflux medium. Results indicate that the GO-Fe2O3-SO3H is the best catalyst for the esterification reaction. Prepared catalysts were characterized by various techniques like SEM, TEM, EDS, Raman Spectroscopy, XRD, TGA, etc. Since the metal oxide supported sulfonated catalysts show better activity in esterification reactions, these catalysts were used for the conversion of waste cooking oil to biodiesel. The GO-Fe2O3-SO3H catalyst contributed better activity in conversion of waste cooking oil to biodiesel. Obtained biodiesel was characterized by 1H NMR and GC-MS. Physiochemical properties of biodiesel were also evaluated. Obtained results were in accordance with the test limits of ASTM. The GO-Fe2O3-SO3H catalyst was reclaimed by magnetic separation and recycled for seven cycles. The TGA curve of the recycled catalyst indicated that the catalyst remained stable up to seven cycles. Thus validating the GO-Fe2O3-SO3H catalyst a green catalyst.ThesisItem Open Access Method development and validation of fluoroquinolones residues in poultry meat by HPLC(DEPARTMENT OF CHEMISTRY SAM HIGGINBOTTOM UNIVERSITY OF AGRICULTURE, TECHNOLOGY AND SCIENCES PRAYAGRAJ - 211007 (U.P.) INDIA, 2019) Sharma, Rajeev; Lawrence, Dr. (Mrs.) Reena S.Analytical methods were developed and validated for the simultaneous determination of selected fluoroquinolones in poultry meat by liquid chromatography. Rapid, simple and sensitive sample treatment procedures were developed and used in order to extract the fluoroquinolones from the chicken tissues with good recoveries. The limits of detection (LOD) and limits of quantification (LOQ) for fluoroquinolones in chicken tissues were well below the Maximum Residual Limits (MRLs) for antibiotics. The separation results and other validation parameters (Linearity, Range, Precision, Intermediate precision, Repeatability, Inter and intraday, Separation, Specificity and Robustness) of the methods were evaluated from spiked tissue samples and results were found good and within range. The proposed methods can be applied for routine determination of the fluoroquinolones in chicken tissue samples. An analytical method using high performance liquid chromatography was developed and validated for simultaneous analysis of residues of danofloxacin and difloxacin in chicken meat. The drugs were extracted from homogenized tissues using amine buffer, followed by extraction with acetonitrile. The separation was achieved by reversed phase chromatography on a C-18 column (250mm x 4.6mm i.d., 5μm) held in thermostat at 30°C. The mobile phase consisted of a mixture of triethyl amine (pH 3.5) and acetonitrile (80:20, v/v), with a flow rate of 0.600 ml/ min. The analytes were detected using PDA detector at the wavelength of 280 nm. The retention times for danofloxacin and difloxacin were about 8 and 15 minutes, respectively. An excellent linearity was revealed in the investigation concentration range from 10 to 1000 ng/ml with correlation coefficients of the curve over 0.99 for both analytes. Recoveries from chicken tissues ranged from 91 to 97% and the limits of quantification for danofloxacin and difloxacin were 35 and 40 μg/Kg in chicken tissues. An analytical method using high performance liquid chromatography was developed and validated for simultaneous analysis of residues of ciprofloxacin and enrofloxacin in chicken meat. The drugs were extracted from homogenized tissues using phosphate buffer, followed by extraction with acetonitrile. The separation was achieved by reversed phase chromatography on a C-18 column (250mm x 4.6mm i.d., 5μm) held in thermostat at 30°C. The mobile phase consisted of a mixture of potassium phosphate (pH 3.25) and acetonitrile (75:25, v/v), with a flow rate of 0.500 ml/ min. The analytes were detected using PDA detector at the wavelength of 277 nm. The retention times for ciprofloxacin and enrofloxacin were about 10 and 13 minutes, respectively. An excellent linearity was revealed in the investigation concentration range from 10 to 1000 ng/ml with correlation coefficients of the curve over 0.98 for both analytes. Recoveries from chicken tissues ranged from 88 to 94% and the limits of quantification for ciprofloxacin and enrofloxacin were 35 and 30 μg/Kg in chicken tissues. An analytical method using high performance liquid chromatography was developed and validated for simultaneous analysis of residues of ofloxacin and pefloxacin in chicken meat. The drugs were extracted from homogenized tissues using amine buffer, followed by extraction with acetonitrile. The separation was achieved by reversed phase chromatography on a C-18 column (250mm x 4.6mm i.d., 5μm) held in thermostat at 30°C. The mobile phase consisted of a mixture of triethyl amine (pH 4.5) and acetonitrile (85:15, v/v), with a flow rate of 0.750 ml/ min. The analytes were detected using PDA detector at the wavelength of 282 nm. The retention times for ofloxacin and pefloxacin were about 7 and 10 minutes, respectively. An excellent linearity was revealed in the investigation concentration range from 10 to 1000 ng/ml with correlation coefficients of the curve over 0.97 for both analytes. Recoveries from chicken tissues ranged from 87 to 97% and the limits of quantification for ofloxacin and pefloxacin were 35 and 30 μg/Kg in chicken tissues.ThesisItem Open Access Evaluation of essential oils of selected spices as food preservatives(DEPARTMENT OF CHEMISTRY SAM HIGGINBOTTOM UNIVERSITY OF AGRICULTURE, TECHNOLOGY AND SCIENCES, 2019) Singh, Ritika; Lawrence, Dr. ReenaThe present study evaluates the in-vitro study to analyze, separate and purify different chemical constituents, antioxidant activity, antibacterial activity and preservation potential of essential oil of Zingiber officinale (ginger), Syzigium aromaticum (clove)and Cinnamomum zeylanicum (cinnamon). The constituents of these essential oil were analyzed by GC/MS technique. The major chemical constituent in Zingiber officinale (ginger) essential oil is β- sesquiphellandrene (6.27%) whereas β-linalool (3.89%) is present as the minor constituent. The major chemical constituent in Syzigium aromaticum (clove) essential oil is eugenol (44.95%) whereas acetyl eugenol (3%) is present as the minor chemical constituent. The major chemical constituent in Cinnamomum zeylanicum (cinnamon) essential oil is trans- cinnamaldehyde (29.05%), whereas triflouro-α-terpineol (3.1%), is present as the minor chemical constituent. Five chemical constituents were isolated from these essential oils. The isolated constituents were camphene, citral, eugenol, β - caryophyllene and trans - cinnamaldehyde. The antioxidant activity of these essential oils were determined by four methods – DPPH (1,1 – Diphenyl-2-picryl hydrazyl free radical) assay, reducing power activity assay, nitric oxide radical scavenging assay and β-carotene bleaching assay. Gallic acid and B.H.T were used as standard. The growth of various pathogenic microorganisms (Escherichia coli, Klebsiella pneumoniae, Pseudomonas aeruginosa, Staphylococcus aureus) were inhibited by these essential oils. The preservation potential was also tested and it was found that the bacterial colony growth was inhibited by these essential oils.ThesisItem Open Access SYNTHESIS OF TRIAZOLE DERIVATIVES AND THEIR BIOLOGICAL APPLICATIONS(SAM HIGGINBOTOM UNIVERSITY OF AGRICULTURE , TECHNOLOGY & SCIENCES ALLAHABAD – 211007, U.P, (INDIA), 2019) SINGH, NEELOTTMA; Chattree, Dr. AmitThe diversity of chemical structures of the 1,2,3-triazole family and their useful biological activities made these compounds attractive targets in synthetic organic chemistry. In the present, work derivatives of triazole were synthesised. The structure of the synthesised triazoles was elucidated by FTIR, 1H NMR and 13C NMR techniques. All spectral data were found in accordance with the assumed structures. The IR spectra of these compounds showed moderately strong bands around 3100-3360 cm-1, 1600-1650 cm-1 and 1250-1270 cm-1 which is the characteristic of the NH, C=N and C=S groups respectively. In the 1H-NMR spectra, a characteristic signal due to the triazole protons appeared at 10.00-11.00ppm, The signal due to the NH protons appeared at 5.50-5.52ppm and the signals due to the aromatic protons appeared at 6.50-8.40 ppm. The synthesised compounds were evaluated for their in vitro antibacterial and antifungal activity through agar well diffusion method against total of 5 bacterial strains viz. Gram negative E.coli ATCC 25922, K. pneumonia, Enterococcus faecalis, Gram positive P. aeruginosa, S. aureus (ATCC 25323) and of 3 fungal strains viz. C.albicans ATCC 90028, C. tropicalis ATCC 750 and C.krusie. 6-nitro-1-(piperazin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one (7b) was able to inhibit significantly the growth of the E.coli, E.faecalis, K. pneumonia. 6-bromo-1-(piperazin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one (7c) was most potent against S. aureus and P. aeruginosa. Compound 10 d N-(1H-benzotriazol-1-ylmethyl)-N-ethylethanamine was the least active against all bacterial stains. Perusal of activity data showed that compound (7a) 6-bromo-1-(piperazin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one was the most active against C.albicans, (7c) 1-(piperazin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one showed the significant antifungal activity against C.krusie and (8b) 6-nitro-1-(piperidin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one was more effective against C.tropicalis. The synthesised compounds were also evaluated for their antidepressant and anticonvulsant activity on male albino mice. The antidepressant activity was screened by Forced swim test and Tail suspension activity. Drug like compound has been given in the dose of 30 mg/kg i.p. Results of antidepressant activity showed that (7b) [6-nitro-1-(piperazin-1-yl-methyl)-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2- Abstract one] was the excellent antidepressant and N-(1H-benzotriazol-1-ylmethyl)-N-ethylethanamine (10g) was the least active antidepressant among the randomly selected seven compounds. For anticonvulsant activity the electroshock assay in mice was used. To deliver the stimuli, a current of amplitude 12 mA, frequency of 50 hz for 0.2 sec was used. 1H-benzotriazol-1-yl(phenyl)methanone(10a) was most active and 6-bromo-1-methyl-3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2H-indol-2-one (7a) was least active among seven selected compounds.ThesisItem Open Access ISOLATION AND CHARACTERIZATION OF NOVEL PHYTOCONSTITUENTS FROM Jasminum auriculatum STEM AND THEIR ANTIOXIDANT ACTIVITY(Department of Chemistry Faculty of Science Sam Higginbottom University of Agriculture, Technology And Sciences Allahabad – 211 007, 2018) Srivastava, Jyotsana; Prakash, Dr. PoonamJasminum auriculatum is a traditional medicinal plant in India. It is distributed widely in South India and also on dry slopes of the Western Ghats. Each part of the plant has medicinal value and is thus commercially exploitable. The present study comprises isolation and characterization of novel phytoconstituents from Jasminum auriculatum stem and their antioxidant activity. Isolation of compounds was done using crude extracts of Jasminum auriculatum stems. The most important step in the analysis was sample preparation. It involves multi steps including sample collection, drying, grinding and extraction. After extraction open column chromatography was used to separate compounds. Purity of isolated compounds was checked on TLC. Three compounds were isolated from the methanolic extract viz cis - n- Dotriacont- 6-enyl (3”, 4”- dioxymethylene phenyl) - trans, trans - 2’, 4’-pentadienoate, 4-Pentadecanoxy ferulic acid and cis-n-Triacont-20-enoic acid. The structures of these compounds were determined by spectroscopic methods including 1H, 13C and Mass spectroscopy. The antioxidant activity of these compounds was determined by DPPH (1, 1- Diphenyl-2-picryl hydroxyl) assay. The result of antioxidant activity indicated that among all these isolated compounds, 4-Pentadecanoxy ferulic acid (34.62%) possess the highest activity followed by cis - n- Dotriacont- 6-enyl (3”, 4”- dioxymethylene phenyl) - trans, trans - 2’, 4’-pentadienoate (22.85%) and cis-n-Triacont-20-enoic acid (20.08%). From the result of the present study it is concluded that compound 4-Pentadecanoxy ferulic acid can act as a potential antioxidant agent.ThesisItem Open Access Plant Mediated Synthesis Characterization of Metal Nanoparticles and their Biomedical Applications(Department of Chemistry Faculty of Science Sam Higginbottom University of Agriculture, Technology and Sciences Allahabad -211007, (U.P.), India, 2018) DASARI, PRABHAKARA RAO; Anthony, Dr. PrashantAn attempt was made to synthesize Silver, Copper Oxide and Zinc Oxide nanoparticles (NPs) by using Carissa carandas, Nerium indicum and Tecoma stans aqueous, ethanolic and methanolic leaf extracts. The characterization by UV-Visible spectroscopy showed peaks at AgNPs (400 – 450 nm), CuONPs and ZnONPs (250 – 400 nm). Structural analysis by TEM and SEM revealed the average size ranged between 20 and 60 nm for all Silver (Ag), Copper oxide (CuO) and Zinc oxide (ZnO) nanoparticles. The elemental analysis by EDAX suggested formation of Ag, CuO and ZnO NPs. Fourier Transform Infrared spectroscopy analysis revealed the reducing and stabilization of the metal NPs due to flavonoids, tannins and saponins etc. Ag, CuO and ZnO nanoparticles were synthesized using aqueous, ethanolic and methanolic extracts of Carissa carandas, Nerium indicum and Tecoma stans plants. The synthesized NPs were analyzed for their antibacterial activity on gram negative bacterial stains viz Escherichia coli, Klebsiella pneumoniae and Pseudomonas aeruginosa and gram positive bacterial strains Bacillus cereus and Staphylococcus aureus. AgNPs were found to be more effective followed by CuO and ZnO NPs for antibacterial activity. 19 The largest zone of inhibition was observed for AgNPs obtained using methanolic extract of Tecoma stans on Klebsiella pneumoniae (21.7 mm). The Ag, CuO and ZnO nanoparticles synthesized using aqueous extracts of Carissa carandas, Nerium indicum and Tecoma stans plants were analyzed for their antifungal activity on Aspergillus niger and Candida albicans. For antifungal activity, the decreasing order of effectiveness observed was Ag > ZnO > CuO NPs. Best antifungal activity was observed for AgNPs obtained using aqueous leaf extract of Tecoma stans against Aspergillus niger (17.267 mm). AgNPs synthesized using aqueous leaf extract of Carissa carandas, Nerium indicum and Tecoma stans plants and CuO and ZnO nanoparticles synthesized using the aqueous and ethanolic leaf extract of above plants were also analyzed for their anticancer activity on MCF-7 cell line. Among these best anticancer activity was observed for ZnONPs obtained using aqueous leaf extract of Tecoma stans. Among the Ag, CuO and ZnO nanoparticles; AgNPs were more stable due to small size, shape and also more effective in different medicinal applications.ThesisItem Open Access CHARACTERIZATION AND ANTIOXIDANT ACTIVITY OF ISOLATED PHYTOCONSTITUENTS FROM PEAR (Pyrus pyrifolia)(Department of Chemistry Faculty of Science Sam Higginbottom University of Agriculture, Technology And Sciences Allahabad- 221007 2018, 2018) Upadhyay, Ms. Pooja; Prakash, Dr. PoonamPear (Pyrus pyrifolia) fruit is popular among consumers due to its high nutritive value and good taste. The aim of present study was to characterize the isolated phytoconstituents from pear pulp and peel and evaluate their antioxidant activity. Repeated chromatography of the extracts on silica gel columns using different solvent systems afforded three pure compounds. The compunds named as oleiyl-β-D-hexaglucoside, oleiyl-β-D-tetraglucoside and (Z) icos 9-enoic acid were isolated from methanol pulp, acetone pulp and methanol peel extracts respectively. All three purified compounds were characterized on the basis of 1H and 13C NMR spectroscopy. The antioxidant potentials of compounds were measured by 2, 2-diphenyl-2-picrylhydrazyl (DPPH) and reducing power assays. The compound isolated from peel extract of the fruit showed maximum scavenging activity than the other two compounds.