Vol. 18(10) October 2014
RP-HPLC method for simultaneous estimation of Metformin
HCl and Pioglitazone in tablet dosage form
Keni S. and Ambadekar S.
The present work describes a validated reverse phase
high performance liquid chromatographic method for simultaneous estimation of Metformin
HCl and Pioglitazone in tablet formulation. Chromatography was performed on a Zorbax
Eclipse C18 (5 cm×2.1 mm I.D) column from agilent in isocratic mode with mobile
phase containing acetonitrile: buffer pH 3.0 (20:80). The flow rate was 0.5 ml/min
and the eluent was monitored at 218 nm. The selected chromatographic conditions
were found to effectively separate Metformin HCl (RT- 0.928 min) and Pioglitazone
(RT- 5.81 min). Linearity for Metformin HCl and Pioglitazone was found in the range
of 800-1200 µg/ml and 24-36 µg/ml respectively. The proposed method was found to
be accurate, precise, reproducible and specific and can be used for simultaneous
analysis of these drugs in tablet formulation.
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Bio-sorption Analysis of Aqueous solution of Cu(II)
by Zea Maize Cob Powder
Kumari Sharda, Virvadiya Chandresh and Gupta Vikal
An attempt has been made to study bio-sorption of copper(II)
ions from aqueous solution by Zea Maize Cob powder using batch adsorption technique.
Zea Maize plant is locally available in sub-humid southern plane and Arawali hills
zone of Rajasthan. The effect of various parameters like adsorption mass, pH, particle
size, contact time and copper ion concentration on bio-sorption process has also
been studied. The bio-sorption process of Cu(II) has been tested with Langmuir and
Freundlich models. The maximum removal efficiency of Cu(II) by Zea maize cob powder
has been found 70% at pH 4.
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Manufacture of acid resistant fly ash geopolymer brick
under atmospheric curing
Muduli Surabhi Dipali, Nayak Bansidhar and Mishra Barada kanta
Geopolymers are aluminosilicate based binder manufactured
by activation of a solid aluminosilicate source material at high alkaline pH. In
this research work fly ash, rich in silica and alumina has been used as a source
material for manufacture of building brick through geopolymerization technology
in presence of alkaline base chemicals consisting of anions of O2-, [OH]1-, Cl1-
and [SO4]2- in different concentrations and sodium silicate solution under atmospheric
curing. Then study has been conducted to assess the acid resistance property of
fly ash geopolymer brick. This work consists in the immersion of fly ash geopolymer
brick in solutions of 1% sulfuric acid and 1% hydrochloric acid up to a period of
12 months and evaluation of its resistance in terms of surface corrosion and compressive
strength at 3 months intervals. The geopolymer fly ash brick immersed in 1% H2SO4
solution has no remarkable change whereas in 1% HCl solution, there was no change
in appearance of the brick and did not show any noticeable change in colour and
remained structurally intact though the exposed surface turned slightly softer in
1% sulphuric acid solution for long duration of exposure.
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Comparison between Conventional and Microwave-assisted
Hydrodistillation Methods towards Extraction of Essential Oils from Murraya koenigii
(Curry Leaves)
Azid M.Z, Sukari M.A., Ng R.C. and Ali N.A.
Study on the extraction of essential oils from leaves
of Murraya koenigii had been carried out by conventional hydrodistillation (HD)
and microwave-assisted hydrodistillation (MAHD) methods. Time of the first oil droplet,
percentage yield of the extracted oils and the chemical components of the extracted
essential oils from both methods were compared. The running time for MAHD was set
at one and half hour while running time for HD was 5 hours. The major components
from the essential oils obtained from HD method were β-copaene (41.5%), α-selinene
(10.0%) and α-humulene (8.4%). Meanwhile, major chemical components extracted from
MAHD method were β-caryophyllene (19.5%), terpine-4-ol (17.6%) and linalool (9.8%).
A total of 79.6% of chemical components were identified from essential oil extracted
through HD method while MAHD method was 75.7%. The first oil droplet for HD method
was found to be at 34 minutes and 20 minutes for MAHD method. MAHD is more preferable
method for extracting essential oils from Murraya koenigii as it provides high extraction
efficiency with less time taken.
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Environment friendly sol-gel pre-treatments for corrosion
protection of aluminium alloys
Chawada G. and Dholakiya B. Z.
In this paper, corrosion resistance and adhesion of environmental
friendly silane pre-treatment on aluminium substrate was studied. Coating solution
(Sol) was formulated by using epoxy bis-silane precursor via acid hydrolysis and
condensation reaction at constant solid content, fixed water ethanol ratio. Two
different formulations (Sol 1 and Sol 2) were developed on the basis of epoxy/silane
ratio. The organic-inorganic hybrid films were deposited on aluminium panels by
dip-coating technique, by immersion of sample panels into the sol and their withdrawal
at controlled rate to facilitate desired and uniform film. Films were subsequently
cured at room temperature. Corrosion resistance of the coating was evaluated by
electrochemical impedance spectroscopy (EIS), DC polarisation techniques and neutral
salt spray test. The adhesion behaviour of the coating was investigated by cross
hatch test. Results showed that Sol 2 showed significant improvement in the corrosion
resistance and adhesion of the coating. Silane pr-treatment has excellent adhesion
with substrate and commercial grade epoxy top coat.
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QSAR Model Study on the Fish Concentration Factors
Fan Deling, Liu Jining, Wang Lei and Shi Lili
The aim was to develop a reliable and practical quantitative
structure-activity relationship (QSAR) model validated by strict conditions for
predicting bio-concentration factors (BCF). We built up three QSAR models starting
from 25 chemicals based on linear heuristic method (HM), radial basis function neural
network (RBFNN) and support vector machine (SVM) methods. The selected six descriptors
are the most important physical chemistry properties for the construction of QSAR
model. In the HM method, the value of square of the correlation coefficient r2 is
0.8479, s2 is 0.0474; in the SVM method, the value of the r2 is 0.9351 and s2 is
0.0233 whereas in the BP method, the r2 is 0.7539, s2 is 0.154. The SVM model may
be used for prediction of toxicity, safety and risk assessment of chemicals to achieve
better ecotoxicological management.
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Anti-bacterial activity of tomato glycosides
Li Jian-Guang and Zhang Lu
Glycosides were extracted from green tomatoes with ethanol
as the solvent. The extracted glycosides were purified by an HPD macroporous resin
and a silica gel column, crystallised and then recrystallised to yield white powder.
The minimal inhibitory concentration (MIC) of the extracted tomato glycosides against
Escherichia coli was determined to be 3.54 mg/mL through agar diffusion test. The
effects of pH, temperature and reaction time on the anti-bacterial activity of the
tomato glycosides were investigated. The bacteriostatic effect of the tomato glycosides
was stronger than that of 1.5% sodium benzoate. The tomato glycosides exhibited
the strongest anti-bacterial effect at pH 7.
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Mineralogy and bioavailability of Selected Heavy Metals
in Agricultural Soils
Ngole Veronica Mpode and Ekosse Georges-Ivo
Contamination of soils with heavy metals from agrochemicals
presents a threat to food security and safety in communities depending on these
soils for subsistence. Knowledge of the various factors and properties dictating
metal behavior in agricultural soils is of paramount importance in the management
of such contamination. This study considered the relationship between soil properties
and metal mobility in three agricultural soil types from Botswana and appraised
the role of clay mineralogy in heavy metal (HM) mobility in these soils. The mobility
factor (MF) of metals in the three soils was determined from results of sequential
extraction of HM in the soils. Mean concentrations of Cr, Co, Cu, Mn, Pb and Zn
were highest in the vertisol with values of 127.7 mg/kg, 45.3 mg/kg, 119.4 mg/kg,
476.9 mg/kg, 52.2 mg/kg and 113.0 mg/kg respectively. Though the concentrations
of HM in the vertisol were highest, the availability of these HM as indicated by
values for MF of the different metals in the vertisol was lowest (0.02 – 1.13) whereas
the arenosol with the lowest concentration of HM had the highest values for MF of
most of the metals (0.54 – 13.38). These MF values were higher than those obtained
for the luvisol which ranged from 0.05 to 1.07. The trends in MF did not match the
trends observed in metal uptake by spinach grown on these soils. The observed patterns
in HM mobility in the soils were attributed to the clay content and mineralogical
assemblage the soils.
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Application of Taguchi Optimization Approach for the
Removal of Cr (VI) from Aqueous Solution using Husk of Cajanus cajan
Kaushik A., Chauhan B. S. and Singh A. K.
The present study investigates the use of Husk of Cajanus
cajan (HCC) as a suitable adsorbent for Cr(VI) from aqueous solutions. This study
includes the Taguchi’s Optimization Technique for process parameter optimization.
Taguchi’s approach helps to create a robust design of experiment which is a systematic
methodology to obtain the results that are least affected by the variations (noise)
of the system. In this method, we used statistical tools like signal-to-noise(S/N)
ratio, analysis of variance (ANOVA). The study reveals that optimum response for
the removal of Cr(VI) is obtained at the pH value 1.0, adsorbent dose 0.7 gm/50
ml and 15.5mg/L metal ion concentration. The results of the study also show that
the pH of the solution is the most influential parameter for the adsorption of Cr(VI).
Confirmation experiment was conducted to investigate the successful implementation
of optimum process parameters.
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Separation and quantification of impurities of Desvenlafaxine
Succinate from active pharmaceutical ingredient (API) using reverse phase liquid
chromatography
Harlikar Jayvant Narayan and Amlani Arun Mahendra
High performance reverse phase liquid chromatography
(HPLC) method was developed for quantification of impurities of Desvenlafaxine Succinate
from active pharmaceutical ingredient (API). Desvenlafaxine Succinate and its impurities
were separated using reverse phase gradient HPLC method. The experimental procedure
involved variable wavelength detector (at 225nm), the mobile phases consisting of
mobile phase A of phosphate buffer and mobile phase B of acetonitrile and water
(98:2V/V) used with gradient program. The flow rate of the mobile phase was adjusted
to 1.0mL per minute on an Inertsil ODS 3V, C-8 (250mm x 4.6mm, 5µ size) column.
A calibration curve showed good linearity within the LOQ to 0.2% of the test range
(i.e. 0.2 ppm to 2 ppm). The recovery at LOQ level ranged from 100% to 109% and
the recoveries at 50% to 200% level ranged from 98% to 106%. The % RSD for repeatability
was ≤ 1.5. The solution stability is established till 24 hours. The HPLC method
is capable of detecting all process related impurities which may be present in the
API. The method was validated and from the results obtained it can be concluded
that the method is suitable for the intended purpose of separation and quantification.
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Fluoride Removal Efficiencies of Some Nano and Bulk
Materials
Dutta P.
The removal efficiencies of fluoride by nano and bulk
material of activated charcoal, silica gel and rice husk were studied with four
different fluoride concentrations viz 5.8, 6.5, 7.7 and 8.6 ppm. It has been observed
that the removal efficiency of fluoride by bulk activated charcoal after 1h was
found to be 55.1, 50.7, 46.7 and 40.5 percent for initial fluoride concentrations
5.8, 6.5, 7.7 and 8.6 ppm respectively and the removal efficiency decreases as the
initial concentration increases. Similarly removal efficiency of bulk silica gel
and rice husk after 1h was found to be 38.2, 37.7, 37 and 36.5 percent for silica
gel and 20.7, 19.8, 19.0 and 18.4 percent for rice husk for same initial concentration
5.8, 6.5, 7.7 and 8.6 ppm respectively and the removal efficiency decreases as the
initial concentration increases. The extent to which fluorides were removed by nano
materials viz. activated charcoal, silica gel and rice husk were higher than that
of respective bulk materials. The higher adsorption capacity of nano materials than
bulk materials may be due to increase in surface area at nano level. The adsorption
data of rice husk was tested for Freundlich adsorption isotherm and Langmuir isotherm
model as rice husk is an eco-friendly and cost effective material.
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Effect of organic manure and mineral fertilizers on
passive pool of soil organic matter in a long-term experiment
Verma Gayatri
Soil organic carbon (SOC) is the most important indicator
of soil quality because of its impact on other physical, chemical and biological
indicators of soil quality. To sustain agricultural productivity and environmental
quality it is important to maintain and improve soil quality in continuous cropping
systems. Long-term studies have consistently shown the benefit of manures, adequate
fertilization on maintaining agronomic productivity by increasing C inputs into
the soil. To understand this phenomenon, passive pool of soil organic matter was
studied in Inceptisol in a long term field experiment established in 1997 under
maize-wheat cropping system at Instructional farm, Rajasthan College of Agriculture,
Udaipur under All India Co-ordinated Research Project. The study involved various
doses of N, NP, NPK with FYM, Zn, S and Azotobacter. Continuous application of organic
manure alone and in combination with inorganic fertilizers enriched the soil with
organic carbon, humic acid, fulvic acid and humin content. However, sole application
of fertilizers led to lower organic carbon content. A significant correlation of
passive fractions of organic matter was obtained with soil properties which revealed
that these help in nutrient recycling and transformation.
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Spectroscopic Investigations on Structural Characterization
of Borate Glass Specimen doped with Transition Metal Ions
Thirumaran S. and Sathish K.
Infra-Red spectroscopy is an effective tool for resolving
the structure of local arrangement in glasses. Infrared investigations reveal structural
changes and observed changes in infrared spectra due to irradiation and can be interpreted
by assuming that irradiation of glass leads to formation of induced defects which
led to decrease of the intensity of the main characteristic mid absorption bands.
Structural changes after irradiation have been investigated by using FTIR spectroscopic
studies. According to IR analysis, there is a depolymerization of the borate network
and conversion of BO3 or BO4 units with the formation of non-bridging oxygen. The
FTIR spectral studies confirm the presence of various functional groups of the sample.
FTIR spectrum of sample exhibits broad absorption bands indicating the wide distribution
of borate structural units. The effect of Na2CO3 and V2O5 and MnO2 contents on the
structures of borate glass is evaluated from the FTIR spectra.
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Biodegradation of polyethylene (HDPE) by Pseudomonas
sp. NCIM 2303
Gaikwad Bhaskar G. and Varma Rita J.
Cultures from NCIM culture collection (National Chemical
Laboratory, Pune, India) were screened for biodegradation polyethylene carry bags.
A strain of Pseudomonas sp. NCIM 2303 was found to be most effective. A film of
polyethylene bag put in the supernatant of cell culture broth showed 4.16 % degradation
in 5 days as determined by weight loss. Studies were carried out to enhance the
biodegradability of the enzyme in the supernatant. It was assumed that after 5 days
the enzyme in the broth is deactivated and hence no further degradation occurs.
Thus after 5 days the film was removed, its weight loss noted and then once again
suspended in fresh culture broth for 5 days, this was repeated until no further
degradation was observed. After 7 cycles a total loss of 23.52 % was achieved.
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