Research Journal of Chemistry and Environment

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Vol. 23(9) September 2019

One step hydrothermal synthesis and characterization of silver nanoparticles

Porwal Dipiti, Prasad Jagdish, Shukla Rachana and Srivastava Krishna

Page No. 1-3

The silver nanoparticles are synthesized by a facile one pot hydrothermal method at 100oC. The study presents the role of reaction parameters in the formation and growth of silver nanoparticle through a synergetic reduction approach using different concentration of precursor materials. The synthesized samples have been characterized by Transmission Electron Microscopy (TEM) and Dynamic Light Scattering (DLS) to study the shape and size of nanoparticles. These nanoparticles exhibit an intensive surface plasmon resonance in the wavelength range of 420- 435 nm in the UV-vis spectrum depending on their shape and size, which make them useful for optical probes, ionic sensing and biochemical sensors. The analysis conducted in this clearly shows that the ratios of precursor material greatly influence the particle size characteristics.

Separation of Ethyl Acetate Fraction of Mengkudu Fruit (Morinda citrifolia L.) and its Hypoglycemic Activity by Glucose Tolerance Method

Shintia Lintang Charisma, Yasmiwar Susilawati, Ahmad Muhtadi and Asman Sadino

Page No. 4-9

Mengkudu (Morinda citrifolia L.) is one of the Rubiaceae medicinal plant that has been used traditionally for lowering blood glucose level. Previous research showed that ethanolic extract and ethyl acetate fraction gave significant hypoglycemic activity. The ethanolic extract of mengkudu fruit at a dose of 300 mg/kg b.w can increase plasma insulin levels in the group of diabetic rats induced streptozotocin 12.52 μU/mL, while the group was given glyclazide (dose 5 mg/kg bw) of 13.27 μU/mL. The ethyl acetate fraction of mengkudu fruit also gave the best hypoglycemic activity (54.29%) followed by n-hexane fraction (34.18%) and water fraction (47.42%). at dose of 1200 mg/kg body weight on male Wistar rats. The aim of this study was to determine the hypoglycemic effect of ethyl acetate subfraction which was separated from ethyl acetate fraction by liquid vacuum chromatography. Subfraction which shows the strongest hypoglycemic effect, indicates that the subfraction contained hypoglycemic active compounds.

Based on TLC profile, the subfractions were grouped into five subfractions (Mc-II-A, Mc-II-B, Mc-II-C, Mc-II-D and Mc-II-E). The hypoglycemic effect of subfractions was evaluated on male mice by glucose tolerance method at a dose of 150 mg/kg body weight. Blood glucose level was measured at 30, 50, 90, 120 and 150 minutes after administration of subfractions. The subfractions Mc-II-A, Mc-II-B, Mc-II-C, Mc-II-D and Mc-II-E showed hypoglycemic effect at 150 minutes with reduction in relative blood glucose levels as 39.11%, 52.85%, 35.31% 43.55% and 33.78% respectively. The study showed that Mc-II-B subfraction indicates the highest hypoglycemic activity by glucose tolerance method.

The antibacterial and anticancer test of cyclomulberochromen compounds from Artocarpus altilis

Tati Suhartati, Gabriella S. Wulandari, Yandri and Sutopo Hadi

Page No. 10-16

One flavonoid compound, cyclomulberochromen (1) has been isolated from the wood branch of Artocarpus altilis. This compound has been physically and spectroscopically determined and tested for bioactivity against Bacillus subtillis and Escherichia coli, it showed strong activity and in cytotoxics test using murine leukemia P-388 cells, was very active.

Factorial optimization of phytase enzyme from Aspergillus ficuum MTCC 7591

Deepika K., Radha K.V. and Manissha S.D.

Page No. 17-22

This research work focuses on the factorial optimization of phytase enzyme from Aspergillus ficuum MTCC 7591. The enzyme hydrolyzes phytic acid present in the plant and also consequently increases in the phosphorus bioavailability to the monogastric animals and reduces the soil pollution. It is also one of the industrially important enzymes used in feed, food, bakery technology, paper and pulp. Agriculture residual wastes were used as a substrate for the organism to produce phytase enzyme because of its support as a matrix for the organism growth and served as a prosperous proteinaceous nutrient. It could be utilized as a potential source for the production of enzyme by fermentation process.

In this study mixed substrate of coconut oil cake and wheat bran was used for the optimization experiment. The parameters taken for the experiment were carbon, nitrogen, temperature, pH, moisture content and incubation time. Studies reported that glucose and peptone served as a good carbon and nitrogen source for phytase production. Furthermore, the temperature of 30°C, pH of 5 and moisture content of 60% with incubation time of 96 hrs showed maximum activity of enzyme. The partial purification of enzyme showed a specific activity of 53.26 U/ mg with yield of 64.18%.

Solid-Phase Peptide Synthesis of PAKY and PACY and Evaluation of their Antioxidant Properties

Rani Maharani, Christina Marpaung, Safri Ishmayana, Dadan Sumiarsa, Achmad Zainuddin, Nurlelasari, Desi Harneti and Unang Supratman

Page No. 23-28

Antioxidant peptides are important molecules that can neutralize free radical and therefore can prevent and cure chronic diseases. One of natural antioxidant peptides is PAGY tetrapetide which is isolated from the skin gelatin of Amur sturgeon (Acipenser schrenckii). The present study was intended to synthesize the analogue of the tetrapeptide i.e. PAKY and PACY and investigate their antioxidant properties. The synthesis was conducted using solid-phase method with the Fmoc/t-Bu strategy. The synthesis was performed on 2-chlorotrytil chloride resin as solid support and all coupling reactions were assisted by the presence of combined coupling reagent, HATU and HOAt. All the peptides were released from the resin by 95% TFA in water. The crude peptides were then purified by respective RP-MPLC with gradient elution (acetonitrile:water=0:100-90:10; 1 h; 3 mL/min; 254 nm; C-18 (4 g) column) and preparative RP-HPLC with isocratic elution (methanol:water=1.2:8.8; 35 min; 6.25 mL/min; 254 nm; C-18 column) and resulted in 21.4 mg PAKY and 14.2 mg PACY.

The peptide was then analyzed using HR-TOF-MS and confirmed by NMR. The DPPH inhibition assay showed that PAKY and PACY have IC50 values of 1.030 and 1.449 mg/mL respectively. The result of the present study indicates that amine and thiol groups on the amino acid side chain of lysine and cysteine increase antioxidant activity of the peptide as compared to its natural analogue PAGY.

Adsorption of Industrial Dyes Reactive Black 8 and Reactive Yellow 84 by PANI- CuCl2: Kinetics and Isotherm Studies

Lingeswari U.D. and Vimala T.

Page No. 29-37

The photocatalytic adsorption of industrial textile dyes Reactive Black 8 and Reactive Yellow 84 was investigated using metal doped PANI composite. Decolorization of these industrial dyes was affected by different parameters like adsorbent mass, dye concentration, dopant mass, pH and temperature. The morphology was characterized by Scanning Electron Microscope and FTIR technique.

Langmuir isotherm and pseudo-second-order kinetics were found to be the most appropriate models to describe the dye removal by adsorption process. Thermodynamic parameters such as free energy (∆G°), enthalpy (∆H°) and entropy (∆S°) changes were also evaluated.

HbA1c and interleukin-17a level inpatient at risk for metabolic syndrome in Yogyakarta

Aulia Rahim, Akrom and Endang Darmawan

Page No. 38-42

Metabolic syndrome resulted from complex metabolic abnormalities due to obesity, hypertension, dyslipidemia and hyperglycemia. Insulin resistance causes an increase in reactive oxygen species that will increase HbA1c levels. Meanwhile, oxidative damage leads to a rise of pro-inflammatory resulting in increased interleukin (IL)-17a. This study aimed to investigate the correlation between HbA1c and IL-17a levels in patients at risk for metabolic syndrome. A total of 89 patients at risk for metabolic syndrome who had met inclusion and exclusion criteria and agreed to fill in the informed consent were involved in this cross-sectional study. Determination of IL-17a level used enzyme-linked immunosorbent assay method. The HbA1c determination was performed using plasma glucose mean way.

The correlation between HbA1c and IL-17a levels was analyzed using bivariate correlation test with a 95% confidence level. There was no difference in HbA1c and IL-17a levels in the sample based on smoking behaviour and clinical manifestations of hypertension, hypertriglyceridemia, diabetes mellitus and obesity. Based on sex and age, there was no difference in IL-17a level, but there was a significant difference in HbA1c level. The conclusion of this study showed no correlation between HbA1c and IL-17a levels in patients at risk for metabolic syndrome.

Structural, Morphological and Crystallographic Study of Zinc Ferrite Nanoparticles with respect to Temperature

Sheikh Arifa and Jain Preeti

Page No. 43-46

In the present work we have fabricated ZnFe2O4 nanoparticles by co-precipitation method using thio-glycerol as shape directing agent. The synthesized nanoparticles were calcined at 200°C, 400°C, 600°C and 800°C annealing temperature for four hours respectively at air atmosphere. The structural properties and crystallinity of as prepared nanoparticles were characterized by XRD and SEM techniques.

XRD results show the formation of single-phase crystalline nature of ZnFe2O4 nanoparticles with major (220) (311) (511) and (440) crystallographic plan and particle size was also evaluated under the range of 9-17nm by using Scherrer's formula. Further, the surface morphology was confirmed by SEM analysis where the nanoparticles appeared in spherical shape under the higher temperature. In this work it is confirmed that as the annealing temperature increases, the particles become more crystalline and the size of zinc ferrite nanoparticles increased linearly.

Solid state sensor based on meso-tetra (p-nitrophenyl) porphyrin deposited glass plate for the determination of trace level HCl gas

Gowthaman N.S.K., Muthukumar Palanisamy and Rajakumar Kanthapazham

Page No. 47-52

A novel solid-state sensor based on meso-tetra (p-nitrophenyl) porphyrin (MTNP) deposited glass plate for the detection of HCl gas was developed and described in this study. Initially, the MTNP molecule was synthesized by Lindsey method and characterized by UV-vis and FT-IR spectroscopic techniques. Addition of HCl into the MTNP-DMF solution leads to the protonation of MTNP which is evidenced from the colour change from dark brown to fluorescent green and it was followed by absorption and fluorescence spectral techniques. Protonation of MTNP leads to changes in Soret and Q bands of the porphyrin. Interestingly, deprotonation on MTNP occurs by the addition of trimethylamine into the same solution and the solution turns into its origin.

Further, detection of HCl gas using MTNP deposited glass plate (solid state sensor) was demonstrated. The solid-state sensor was characterized by UV-vis, fluorescence and scanning electron microscopy (SEM). The SEM image shows discrete aggregates after the solid-state sensor was exposed to HCl gas. Detection of HCl gas monitored at 464 nm and the sensitivity of the solid-state sensor were achieved up to 30 ppm. The sensor fails to detect below 5 ppm of the HCl gas and is also slightly affected by humidity.

Removal of Octylphenolethoxylate from Waste Water using Carbonized and Non Carbonized Agro Waste of Typhalatifolia

Khandelwal Arundhati and Agrawal Manisha

Page No. 53-61

Removal of higher concentration of nonionic surfactant Octylphenolethoxylate with 10 moles of ethylene oxide (OPE-10) trade name, Octylphenolethoxylate from industrial effluents, using the carbonized stem of aquatic weed Typhalatifolia, has been discussed in the present investigation. Carbonization of Typhalatifolia stem was done in the laboratory by using Muffle furnace instrument at temperature 500oC. The removal of surfactant is calculated by U-V spectrophotometer using cobalt thiocyanate active substances (CTAS) method. Various concentrations of surfactant solutions in the range from 200ppm to 1000ppm have been prepared for extraction work.

Optimization of the experiments is done by calculating variables – shaking time, doses of absorbent bed and concentration of reagents. Degree of adsorption is validated and compared with isotherm models of Langmuir adsorption isotherms, Freundlich adsorption isotherms, Temkin adsorption isotherms Dubinin-Radushkevich adsorption isotherms and Harkin Jura isotherms. R2 value among all isotherms best suited is Freundlich adsorption isotherm. SEM images of non-carbonized and carbonized agro-waste are also analyzed and compared. The variance of ANOVA was considered significant at p = 0.25.

Lutetium-177 separation from irradiated natural ytterbium using extraction-column chromatography method after reduction by magnesium

Setiawan Duyeh, Febrian Basit M., Setiadi Yanuar, Hastiawan Iwan and Larasati Tiara

Page No. 62-67

177Lu radioisotope is obtained as decay product of radioisotop 177Yb from neutron irradiated natYb. The aims of this project were to get the optimum conditions of 175/176Yb/natYb reduction and to separate 177Lu from 176Yb along with the analysis of its purity. natYb was irradiated under neutron thermal on nuclear reactor TRIGA 2000 Bandung at neutron flux >1013 n.cm-2.s-1 for 4 days. Irradiated natYb was reduced using magnesium reducing agents with variations in the number of moles. Separation of 177Lu-175/176Yb/natYb was carried out through column chromatography extraction method based on the LN Eichrom resin matrix with HNO3 solution as an eluent. Radiochemical purity of eluant 177Lu(NO3)3 was determined by using paper chromatography method and radionuclide purity of eluant was measured by spectrometer gamma with multichannel analyser.

The results of this research showed that the optimum reduction conditions were found at the mol ratio of 1: 8 (Yb: Mg). Percentage of 177Lu-175/176Yb/natYb separation was obtained at 32.18 ± 0.34% in the addition of thioglycolic acid and HNO3 eluant at concentrations between 2 - 4 M at the flow rate of 0.5 mL/ minute. The final product in the chemical form of 177Lu(NO3)3 clear solution, pH 2, radiochemical purity of 89.81 ± 0.82% and radionuclide purity was greater than 99%.

Synthesis and spectral studies of Macrocyclic Ni (II) Complexes with Multidentate ligands

Kumar Raman

Page No. 68-70

The complex of NI(II) with multidentate Schiff base ligand H2 (Mahe1-2) derived from the reaction between Diacetylmonoxime and 1, 3 – Diaminopropane or, 1, 4 – Diaminobutane in dry alcoholic medium have been synthesized and characterized on the basis of elemental analyses, magnetic susceptibility, infrared, electronic spectral and conductivity data. The metal chelates ligand have a general formula Ni (H2 Mahe1-2). IR spectral data suggest that the ligand H2(Mahe1-2) behaves as endo quadridentate ligand. The electronic spectral and magnetic susceptibility measurement indicate diamagnetic behaviour of endo quadridentate square planar geometry around the Nickel centre with Bis- (oxime) amine unit coordinating in a facial mode.

The stability of the macrocyclic complex has been found to be dependent on the ring size of the cavity of the macrocyclic ligands which can be varied by changing the number of intervening atoms between two-amino groups in the terminal and intramolecular hydrogen bonding.

Adsorptive removal of Crystal violet dye from aqueous solution using activated carbon prepared from Cassia fistula (L) fruit shell

Savithri S., Rajeshwari M., Nandhakumar V., Durgadevi K. and Chandramohan M.

Page No. 71-75

Activated carbon was prepared from the fruit shell of Cassia fistula (L) by sulphuric activation method and designated as Cassia fistula Fruit shell Carbon (CFC). Adsorption potential of CFC is studied with Crystal violet (CV) dye as adsorbate using its synthetic aqueous solution. Effect of solution pH, CFC dose, contact time, initial concentration of CV dye and temperature was investigated. Desorption study was also performed.

It was noted that CV dye uptake per unit weight of CFC increased with increase of a CV dye concentration, increase of CFC dose and temperature. Above study revealed that adsorption of CV dye onto CFC was physisorption and endothermic nature. As Cassia fistula (L) fruit shell is discarded as waste material, CFC is expected to be economical product for CV dye removal from water.

A Novel Pyrimidine compound Ethyl-4-(2,4-dichlorophenyl)-1,2,3,4-tetrahydro-6-methyl-2 thioxopyrimidine-5-carboxylate as an Efficient Antioxidant agent

Pasupathi M., Santhi N., Manivannan C., Viswanathan G. and Pachamuthu M.P.

Page No. 76-82

The pyrimidine-based derivatives are known for their applications in medicinal chemistry (antibacterial, anti-depressant, anti-platelet, anti-hypersensitive and anti-inflammatory). Many functional/molecules substituted pyrimidines are developed recently. The present work reports on the synthesis of Ethyl-4-(2,4-dichlorophenyl)-1,2,3,4-tetrahydro-6-methyl-2-thioxo pyrimidine-5-carboxylate (DCPC), different groups modified pyrimidine compound using a novel, three dimensional, aluminium (Al) and titanium (Ti) modified nanoporous heterogeneous catalyst AlTiTUD-1.

The structure of synthesized DCPC compound was confirmed by nuclear magnetic resonance (NMR) and Fourier transform infrared (FT-IR) spectral analysis. The antioxidant activity of the novel compound was probed using 1,1-diphenyl-2-picryl-hydrazyl (DPPH), Hydrogen peroxide (H2O2), 2,2’-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid (ABTS), nitric oxide (NO•) and hydroxyl radical (•OH) scavenging assays. The compound showed significant radical scavenging potential.

Steroid Koenol from the Leaves of Murraya koenigii Spreng

Josewin B., Divya Mohan, Simi V.K. and Remya T.S.

Page No. 83-87

The dried powdered leaves of Murrayakoenigii Spreng were extracted successively with ethyl acetate and aqueous methanol. The ethyl acetate soluble part on column chromatography gave one compound whereas aqueous methanol soluble part gave four compounds. The isolated compounds were identified by spectroscopic methods and found to be a steroid compund1koenol from ethyl acetate extract and four compounds namely 2. Curryanine 3. Curryangine 4. lup-20(29)-en-3-β-ol and 5. 3-palmityl-24 R-stigmast-5-en-3-β-ol from aqueous methanol extract.

Partial Purification and Characterization of Xylan degrading Alkaline Xylanase from Bacillus subtilis

Shekhar Sudhir Kumar, Ahmad Abrar, Godheja Jai and Modi Dinesh Raj

Page No. 88-93

Microbial Xylanases have important applications in the degradation of xylan. Alkaline Xylanase from Bacillus subtilis, an effective thermophilic bacterial strain, was selected with a goal to accomplish the Xylanase production. The effective Xylanolytic strains of Bacillus subtilis required an optimum temperature of 50°C for 72 hrs for maximum Xylanase production. The optimum pH and Xylanase concentration observed were 7.0 ± 0.2 and 1.0 % respectively. Media with 1% maltose as carbon source, NH4NO3 as inorganic nitrogen source and CuSO4 as mineral salt were found best to enhance the production of Xylanase.

In Maximum yielding conditions, Xylanase produced by Bacillus subtilis was purified by precipitation with ammonium sulfate at 60% saturation which showed a specific activity of 12.65 µg/mg. Xylanase was purified to 1.9 fold with approximately 9.2% recovery. The enzyme was further subjected to dialysis which yielded highest specific activity of 26.02 µg/mg. The enzyme was finally purified with column chromatography to 3.9 fold with 6.7% recovery. Purified Xylanase was used for determining effects of pH, temperature and metals on enzyme activity. Maximum enzyme activity was reported at pH 7.0 (3.31 µg/ml) and 8.0 (3.35 µg/ml) and maximum enzyme activity (1.4 µg/ml) was reported at 50°C. Highest effects of metals on enzyme activity were found in FeCl3 (4.12 µg/ml). Isolated Xylanase has potential to be used in large scale at Industrial level.

Isotherm analysis on the removal of safranin dye using acid activated hibiscus sabdariffa stem nano carbon

Manivannan P., Arivoli S. and Mohamed Raja

Page No. 94-100

The aim of the present work was to investigate the removal of Safranin dyes from aqueous solution by using Hibiscus Sabdariffa Nano Carbon (AHSNC). Generally, dyes are organic compounds used as coloring products in chemical, textile, paper, printing, leather, plastics and various food industries. In this study, Hibiscus Sabdariffa plant was studied for its potential use as an adsorbent for removal of a cationic dye Safranin.

The various factors affecting adsorption such as initial dye concentration, contact time, adsorbent dose and effect of temperature were evaluated. The experimental data were fitted into the pseudo-second order kinetic model. The equilibrium of adsorption was modeled by using the Langmuir and Freundlich isotherm models. AHSNC may be utilized as a low-cost adsorbent for Safranin dye removal from aqueous solution.

Evaluation of antibacterial activity of iron nanoparticles treated with Mukia scabrella and Solanum xanthocarpum leaf extracts

Sahana S., Dharani T., Tamilselvi S. and Sudarshana Deepa V.

Page No. 101-107

The present study envisioned the green synthesis of iron nanoparticles (FeNP) from leaf extracts of Mukia scabrella and Solanum xanthocarpum. The FeNP synthesized was confirmed by color change to brownish grey color. The obtained FeNP was further validated by the UV absorption spectroscopy and showed peak at 440nm as standard reference. The morphology and crystalline structures of FeNP were determined by SEM and XRD analysis.

The FTIR spectroscopy analysis authenticated the attachment of bioactive plant molecules on iron nanoparticles. Furthermore, the antibacterial activity of FeNPs was screened against bacterial pathogen Escherichia coli, Staphylococcus aureus and Bacillus subtilis. The results showed a significant inhibition of FeNP against pathogens. This result may pave a way for the using of green synthesized magnetic nanoparticles in biomedical and pharmaceutical industries.

Synthesis, Identification and Biological Activity of some Schiff Bases derived from 1,5-diamino naphthalene substrate

Shireen Mohammed, Alya Dawood and Mohammed Mohammed

Page No. 108-112

New Schiff base compounds have been prepared. Various aliphatic and aromatic ketones were condensed with naphthalene-1, 5-diamine to yield the desired Schiff bases. The structures of all the new products obtained in the present work are supported by spectral and analytical data (IR, NMR and Mass spectroscopy).

Furthermore, the biological activity of Schiff Bases compounds was tested against two types of bacteria gram positive for the dye (Staphylococcus aureus) and gram-negative dye (E.Coli).

Phytochemical Screening, proximate and elemental analysis of plant species Curcuma caesia, Curcuma longa and Chenopodium album

Tamrakar Vinita, Arora Dhruv and Arora Charu

Page No. 113-117

Plant species namely Chenopodium album, Curcuma caesia and Curcuma longa were screened for presence of phytochemicals namely alkaloid, tannins, saponin, steroid, flavonoid, terpenoid and phlobatannin; trace elements, moisture and ash content.

These studies may be helpful to explore the role of these plant species for development of herbal formulations and agrochemicals. The phytoconstituents and trace elements present in the medicinal plants play important role to treat the various diseases. Energy Dispersive X ray (EDX) technique is used to identify the elemental composition of plant material in the present study.

Tetra acetoxymethyl glycoluril as Precursor in the preparation of Cucurbit[6]uril and New Oligomer

Salah Arrous, Imene Boudebouz and Abdigali Bakibaev

Page No. 118-121

Substituted glycolurils are of considerable interest for the synthesis of cucurbit[n]uril and acyclic oligomer. The present study investigates the synthesis of cucurbit[6]uril from tetra acetoxymethyl glycoluril in the presence of HCl. We also described the formation of new oligomer achieved by using tetra acetoxymethyl glycoluril with HCOOH in water at 100°C for 20 hours. The structure of the new oligomer has been determined by IR, 1H-NMR and 13C-NMR data and ESMS.

Polyvynilpyrrolidone in use of solid dispersion: A Review

Tazyinul Qoriah Alfauziah and Dolih Gozali

Page No. 122-128

Poor solubility and bioavailability of active pharmaceutical ingredients are always the challenges in the development of efficient drug formulation. Several technologies can be used to improve solubility and one of them is solid dispersion. Solid dispersion is one of the most promising strategies in bioavailability improvement of poor-soluble drugs.

Through this technology, the particle size of the drug was reduced; wettability and dispersibility were improved, so the dissolution rate was increased. This study will describe the importance of solid dispersion, methods of preparation of solid dispersion and polyvynilpyrrolidone role as a carrier in solid dispersion system.