Asian Journal of

Research in Chemistry
ISSN 0974-4169(print) 0974-4150 (online) www.ajrconline.org Volume 04, Issue 03, March, 2011

CONTENT

REVIEW ARTICLE
• Oxindoles and Their Pharmaceutical Significance- an Overview
Shashi Ravi Suman Rudrangi, Vijaya Kumar Bontha, Venkata Reddy Manda and Srinivas Bethi……………………………………… 335
• Metallosulpha Drugs: Synthesis and Bioactivity
Vikram Singh, N.K. Kaushik and Ram Singh…………………………………………………………………………………………………… 339

• Iron Determination - A Review of Analytical Methods

Bhavna V. Mohite…….……………………………………………………………………………………………………………………………. 348

• Solid Phase Synthesis and Their Screening System – Review

A.K. Mishra, A. Gupta, A.K. Singh, R. Sannd, P. Bansal, S. Kumar and V. Gupta……………………………………………………….. 362

RESEARCH ARTICLE
• Simultaneous Spectrophotometric Estimation of Thiocolchicoside and Diclofenac Potassium in Combined
Capsule Dosage Form
A.R. Umarkar, Y.M. Bagad, N.S. Rewatkar and L.T. Thote………………………………………………………………………………….. 370

• Confirmatory Method for Determination of 11-Nor- 9 -Tetrahydrocannabinol-9-Carboxylic Acid in Urine

Samples Using Gas Chromatography–Mass Spectrometry (GC/MS)
Rabie S. Farag, Sayed R. Abed Al-Salam……………………………………………………………………………………………………….. 373

• Theoretical Prediction of Reactive Site of Aryl Halide for Suzuki Coupling Reaction
R. Margabandu and K. Subramani…….………………………………………………………………………………………………………… 377

• Synthesis, Thermogravimetric, Microbial Studies of Ligand and its Metal Derivatives

F. Mazher, B. Khan and T. Kazmi……………………………………………………………………………………………………………….. 381

• Comparison of Photodynamic Activities of Ag@Tio2 and Au@Tio2 Core – Shell Nanoparticles in Human
Erythrocytes
Karunakaran Sulochana Meena, Thyagarajan Venkataraman, Prakasa Rao Aruna and Singaravel Ganesan………………………..387

• Sorption of Chromate and Arsenate by Surfactant Modified Zeolite

Vandana Swarnkar, Radha tomar and Nishi Agarwal……..…………………………………………………………………………………..392

• Physico Chemical Properties of the Sewage Water Used for Growing Certain Vegetable Crops in Etmadpur
Area of Agra Region
Preeti Parashar, F.M Prasad, Shashank Sharma and Jolly Singh……..……………………………………………………………………. 399

• Influence of Chloride Ion on the Corrosion Inhibition Efficiency of the ATMP - Zn 2+ System
C. Thangavelu, P. Patric Raymond, S. Rajendran and M. Sundaravadivelu…….…….…….…….…….…….…….…….…….…………402

• Analysis of Midazolam in Small Volumes of Plasma Using High Performance Liquid Chromatography and
UV-Detection Method: Pharmacokinetics of Midazolam in Rats
Swapnil J. Dengle, Shriram M. Pathak, Chandra Mohan, Arumugam Karthik, Prashant Musmade, Krishnamurthy Bhat and
Nayanabhirama Udupa…………….…….…….…….…….…….…….…….…….…….…….…….…….…….…….…….…….…….………. 406
• Simultaneous Estimation of Cefixime and Ofloxacin by Derivative Spectroscopy Method
S. A. Shah, M. P. Vaghela, B. P. Marolia and K. L. Daxina. ………………….…….…….…….…….…….…….…….…….…….……….415
• Interference Study on Artificial Sweeteners in Forensic Toxicological Screening by TLC
Mohd Idris, S.K. Shukla and T.R. Baggi………..…….…….…….…….…….…….…….…….…….…….…….…….…….…….………….. 419

• Synthesis and Biological Evaluation of 1-Naphthyl and 4-Biphenyl Derivatives of 2, 4, 5-Trisubstituted-1H-

Imidazoles as Antibacterial and Antifungal Agents.
S.D. Sawant, R.N. Patil and A.A. Baravkar…………….…….…….…….…….…….…….…….…….…….…….…….…….…….………... 423

• Studies on Ethanol Production from the Fruit Waste Using Ultrasound Assisted Fermentation
Mahesh S. Patil and Shrikant R. Kulkarni…………….…….…….…….…….…….…….…….…….…….…….…….…….…….…….…… 429

• RP-HPLC Method for the Estimation of Atorvastatin Calcium in Bulk and Pharmaceutical Formulations
P. Nagaraju, B. Sridhar, P. Jitendra Kumar, U. Upendra rao, K. Hanumantha Rao and P.N.V. Gopal……..…….…….…….………434

• Development and Validation of Stability Indicating HPTLC Method for Determination of Trandolapril as
Bulk Drug
Sejal P. Gandhi, Mohit G. Dewani, Tejas C. Borole and Mrinalini C. Damle…………….…….…….…….…….…….…….…….……..437

• Synthesis of Indophenazino Fused Azacarbazole Derivatives of Biological Interest

Veena Yadav and Nishant Yadav………..…….…….…….…….…….…….…….…….…….…….…….…….…….…….…….…….……….441

• Terminalia chebula Retz. Stem Bark Extract: A Potent Natural Antioxidant

Jiby Elias, Rajesh M.G., Anish N.P., Manu M.S. and Iwin C.V………..…….…….…….…….…….…….…….…….…….…….………...445

• In Vitro Anti Oxidant Study of Ethanolic Extract of Coldenia procumbens Linn

Beena P., Purnima S. and Kokilavani R…………….…….…….…….…….…….…….…….…….…….…….…….…….…….…….……… 450

• Nutritional Potentials of Rhynchophorus phoenicis (Raphia palm weevil): Implications for Food Security
A. J.Chinweuba, I. E. Otuokere, M.C. Opara and G.U. Okafor……..…….…….…….…….…….…….…….…….…….…….…….……. 452

• Synthesis and Antimicrobial Activity of Mannich Bases of 1-Isonicotinoylpyrazolidine-3, 5-Dione

Sudhir Bharadwaj, Bharat Parashar, Dimple K. Rathore and V.K. Sharma………...……..……..……..……..……..……..……..…….. 455

• Comparative In vivo Evaluation of Propranolol hydrochloride following Oral and Transdermal

administration in Rabbits
V. Sai Kishore, T. E. Gopala Krishna Murthy and C. Mayuren……...……..……..……..……..……..……..……..……..……..………… 461

• Evaluation of Citrillus vulgaris (Watermelon) Seed Oil As a Source of Alternative Energy to Diesel Oil
A.J. Chinweuba, I.E. Otuokere, M.C. Opara3 and G.U. Okafor……….……..……..……..……..……..……..……..……..……..………. 466

• Kinetics and Mechanism of Micelle-Catalysed Oxidation of DL-Alanine and Glycine by Chloromine-T

Farhat Hasan Khan and Mahboob Alam……….……..……..……..……..……..……..……..……..……..……..……..……..……..……….468

• Study on Ground Water Quality of Greater Visakhapatnam City, Andhra Pradesh from July, 2007 to June, 2008.
G.Srinivas Rao and G.Nageswara Rao…….……..……..……..……..……..……..……..……..……..……..……..……..……..……..……..481

• Manganese (II, III, IV) Complexes of N-(2-Hydroxysalicyliden-1-Yl) Methyleneben- Zoylhydrazide;

Synthesis and Spectral Studies
Nirmal K. Kar………...……..……..……..……..……..……..……..……..……..……..……..……..……..……..……..……..……..……..….. 491

• Stability Indicating HPLC Method for Simultaneous Determination of Repaglinide and Metformin
Hydrochloride in Pharmaceutical Dosage Form
Deepa R. Patel, Laxmanbhai J. Patel and Madhabhai M. Patel……….……..……..……..……..……..……..……..……..……..………. 500

• Instruction to author …………………………………………………………...………………………………………………. 506

 Abstract
REVIEW ARTICLE
Oxindoles and Their Pharmaceutical Significance- an Overview
Shashi Ravi Suman Rudrangi, Vijaya Kumar Bontha, Venkata Reddy Manda and Srinivas Bethi…………………...335

ABSTRACT:
Oxindoles are credited to have a wide range of applications and are reported to exhibit an extensive range of
biological effects which include the antiviral, antifungal, antibacterial, antiproliferative, anticancer, anti-
inflammatory antihypertensive and the anticonvulsant activities. The chemistry of oxindoles is very interesting and
the biological activity of the oxindoles and their derivatives has made them very important in synthetic organic and
medicinal chemistry. This review provides insight into various applications of oxindoles and their derivatives to
date.

KEYWORDS: Oxindoles, Oxindole derivatives, Applications, Biological Activity

Metallosulpha Drugs: Synthesis and Bioactivity

Vikram Singh, N.K. Kaushik and Ram Singh………………………………………………………………………………...339

ABSTRACT:
Compounds containing the sulphonamide group have long been used as drugs for various diseases. The biological
activity of these drugs is enhanced on undergoing complexation with metal ions. This review covers the literature
that has been surveyed to provide a comprehensive coverage of the synthesis and biological activity of
metallosulpha drugs.

KEYWORDS: Sulpha drugs, Metal ions, Metallosulpha drugs, Bioactivity

Iron Determination - A Review of Analytical Methods

Bhavna V. Mohite………………………………………………………………………………………………………………..348

ABSTRACT:
In nature understanding of biogeochemical processes can be done by determining the concentration of soluble
reactive species. Iron is one of the most reactive elements in environments, and its cycling is coupled to other major
biochemical elements like C, O, S, and P along with trace elements such as heavy metals. Iron determination found a
major boon for the various clinical and agricultural activities so in the last 25 years the range for clinical
determination of iron status has been extended with important methods. This review focuses on conventional as well
as recent analytical methods for iron determination and a comparative account of it.

KEYWORDS: Iron, biogeochemical elements

Solid Phase Synthesis and Their Screening System - Review

A.K. Mishra, A. Gupta, A.K. Singh, R. Sannd, P. Bansal, S. Kumar and V. Gupta……………………………………..362

ABSTRACT:
The use of solid phase synthesis techniques has been explored as an alternative to conventional approaches for the
synthesis of compounds used in the drug discovery process. Combinatorial chemistry now plays an important role in
the lead discovery and hit optimization processes in the pharmaceutical world as well as in other areas of discovery
chemistry. Now days this is an important technique for the development of different synthesis concepts that were
intended to cover and explore the chemical space without having to prepare every individual compound. Solid phase
synthesis technologies were developed in response to the increased screening capacities and target oriented lead
finding. This article explains different linker, protecting group, cleavage methods used in solid phase synthesis,
combinatorial libraries and screening system used in solid phase synthesis.

KEYWORDS: Solid phase synthesis, Combinatorial chemistry, Linker, Protecting group.

RESEARCH ARTICLE
Simultaneous Spectrophotometric Estimation of Thiocolchicoside and Diclofenac Potassium in Combined
Capsule Dosage Form
A.R. Umarkar, Y.M. Bagad, N.S. Rewatkar and L.T. Thote………………………………………………………………..370

ABSTRACT:
Two simple, rapid, accurate and economical analytical methods have been developed for the simultaneous
estimation of Thiocolchicoside and Diclofenac potassium in combined capsule dosage form. First method is based
on the determination of Q-value and Second method is based on simultaneous equation method. Thiocolchicoside
has absorbance maxima at 259 nm and Diclofenac potassium has absorbance maxima at 271 nm in distilled water
and phosphate. The absorption ratio (Q-value) was determined at 264 nm (Iso-absorptivity point) and 259 nm (_max
of Thiocolchicoside Both the drugs obey Beer’s law in the concentration ranges employed for these methods. Both
the methods were found to be simple, rapid, and accurate and can be adopted in routine analysis of drugs in
formulations. The accuracy and reproducibility of the proposed method was statistically validated by recovery
studies.

KEYWORDS: Absorption ratio, Simultaneous equation, Overlain spectra, Recovery studies

Confirmatory Method for Determination of 11-Nor- 9 -Tetrahydrocannabinol-9-Carboxylic Acid in Urine

Samples Using Gas Chromatography–Mass Spectrometry (GC/MS)
Rabie S. Farag, Sayed R. Abed Al-Salam…………………………………………………………………………………….373

ABSTRACT:
Gas chromatography mass spectrometry (GC/MS) analysis of 11-Nor- 9-tetrahydrocannabinol-9-carboxylic acid
(THC-COOH) and the major metabolite of tetrahydrocannabinol in biological samples is reported The THC
metabolite obtained by alkaline hydrolysis from urine samples were extracted using mixture of solvents followed by
trimethylsilylation. The derivatized extract was submitted to GC/MS analysis of EI-SIM mode. Different factors
were studied as pH, temperature and time to establish the best conditions for the determination. The calibration
curves of THC-COOH derivatized (THC-COOH-TMS) in urine samples were linear in the concentration range from
10 to 150 ng/ml. The proposed method is able to determine the major metabolite of cannabis derivatives at very low
level (10 ng/ml) with high specificity so is analytical procedure can be used as confirmatory method in drug testing
of cannabis use.

KEYWORDS: Cannabinoids; GC/MS analysis; Tetrahydrocannabinol and Biological samples

Theoretical Prediction of Reactive Site of Aryl Halide for Suzuki Coupling Reaction
R. Margabandu and K. Subramani…….………………………………………………………………………………………377

ABSTRACT:
The aryl c-c bond formation is accomplished via Suzuki coupling by treating aryl boronic acid with aryl halide in the
presence of Pd (0) complexes and base. The reactivity order of aryl halide is I > Cl > Br for Suzuki coupling. If aryl
halide containing different halogen atom as poly substitute, then it does not require any theoretical prediction for
reactive side prediction of aryl halide since we know the order of reactivity but if aryl containing more than one
same halogen atom in that case theoretical prediction will help us to predict the reactive side of aryl halide. In this
work 2,3- dibromo pyridine and 2,5 dibromo pyridine reactivity towards Suzuki coupling is determined by charge
density on bromine atom and bond order between the bromine and carbon atom. The aryl halide bromine atom
having more electron density is readily reacting with Pd(0) complex in oxidative addition step and in the bond order
respect, the aryl halide having smaller value of bond order (carbon halogen bond) is readily reacting with Pd (0)
complex in oxidative addition step. The calculations were done semi-empirical level with PM3 Hamiltonian in RHF
method.

KEY WORDS: Suzuki coupling, oxidative addition, bond order, PM3

Synthesis, Thermogravimetric, Microbial Studies of Ligand and its Metal Derivatives
F. Mazher, B. Khan and T. Kazmi……………………………………………………………………………………………..381

ABSTRACT:
o-Amino-N, N-diethylbenzylamine and its complexes with Cd(II), Pb(II) and Hg(II) metals were synthesized. The
evaluation of complexes was carried out on the basis of infrared and analytical data. The amount of metals was
estimated by atomic absorption spectroscopy. Crystalline nature of complexes was investigated by their XRD
pattern. Thermal behavior of the complexes was studied by Thermogravimetric (TGA) and differential thermal
analysis (DTA) to find out the relative stabilities of the complexes. Antimicrobial activities of complexes were
investigated by diffusion plate method.

KEYWORDS: Synthesis, Thermal analysis, Antimicrobial activity, o-Amino-N,N-diethylbenzylamine.

Comparison of Photodynamic Activities of Ag@Tio2 and Au@Tio2 Core – Shell Nanoparticles in Human
Erythrocytes
Karunakaran Sulochana Meena, Thyagarajan Venkataraman, Prakasa Rao Aruna and Singaravel
Ganesan…………………………………………………………………………………………………………………………387

ABSTRACT:
Core-shell type nanoparticles namely Ag@TiO2 and Au@TiO2 were prepared by one pot simultaneous reduction of
HAuCl4 and hydrolysis of Ti(IV) isopropoxide. They were characterized by absorption and fluorescence
spectroscopy, XRD, HR-TEM and AFM techniques. XRD patterns show the presence of anatase form of TiO2 and
the noble metals. Since the catalytic properties of the oxide surfaces modified with the metal core especially photo
catalysis is an important aspect and considering the fact that erythrocytes serve as model cells to the molecular
mechanism of PDT, the photohemolysis was studied using these core-shell type NPs viz. Ag@TiO2 and Au@TiO2.
Their photodynamic activities were compared. The effect of scavengers viz., GSH and NaN3 showed that there is a
considerable amount of reactive oxygen species formation which are responsible for cell death. The detailed
mechanism has been discussed.

Sorption of Chromate and Arsenate by Surfactant Modified Zeolite

Vandana Swarnkar, Radha tomar and Nishi Agarwal……..………………………………………………………….392

ABSTRACT:
In recent years growth of industries has led to introduction of pollutants in nature, especially the heavy metal ions
like Cr(III) and As(V) usually present in many waste water. Heavy metal containing waste is generated from
industries like metallurgical, mining, chemical, leather, distilleries, sugar, battery, electroplating and pigments.
Chromium is found in natural water in oxidation states Cr(III) and Cr(VI). The former is essential elements for
mammals where as the later is reported to be toxic. Same as arsenic is an ubiquitous contaminant which can be
found at high concentrations in natural waters and wastewaters. Arsenic containing waste streams are generated
mainly by the microelectronic industry and by pesticide and pharmaceutical facilities. It occurs in two oxidation
states that form oxyanions, arsenate As(V), and arsenite As(III); arsenite is more mobile and toxic than AsO4-3. As
arsenic is a major hazardous contaminant for the human health, its removal is an issue of increasing concern. Zeolite
are crystalline, hydrated aluminosilicate containing exchangeable alkaline and alkaline earth cations in their
structural frameworks. Since zeolite have permanent negative charge on their surfaces, they have no affinity for
anions. However recent studies have shown that modification of zeolite with certain surfactants or metal cations
yield sorbents with a strong affinity for many anions. Zeolite has high internal and external surface areas and high
internal and external cation exchange capacities suitable for the surface modification by cationic surfactant
(HDTMA). When the initial surfactant concentration is less than the critical micellar concentration (CMC), the
sorted surfactant molecules primarily form a monolayer, limited chromate and arsenate sorption indicates that the
patchy bilayer may also be formed. When the surfactant concentration is greater than the critical micellar
concentration and enough surfactant exist in the system, the sorbed surfactant molecules form bilayer, producing
maximum chromate and arsenate sorption. Quantitative sorption of chromate and arsenate and desorption of
bromide ions indicate that the sorption of oxoanions is primarily due to surface anion exchange.
KEYWORDS: Sorption; Ion exchange; HDTMA; CMC
Physico Chemical Properties of the Sewage Water Used for Growing Certain Vegetable Crops in Etmadpur
Area of Agra Region
Preeti Parashar, F.M Prasad, Shashank Sharma and Jolly Singh……..…………………………………………………399

ABSTRACT:
In the field experiment conducted in the varying plots in Etmadpur area of Agra region to study the physico
chemical properties of six sewage samples and its effect on vegetable crop. Accumulation of mineral constituents
and heavy metals in soil and vegetable crop like spinach and Okra showed varying results. When the sewage water
samples (W1-W6) were tested the results were that all the samples were found in the range of (7-8 pH).CO3 is found
maximum in 2 samples 2meL-1 (W5-W6), HCO3 is found maximum in one sample 18meL-1 (W2). Cl recorded
maximum in 15 meL-1(W6). None of the samples (W1-W6) were detected suitable for irrigation as all were basic in
nature. The class of irrigated water is found to be basic in nature therefore not suitable for irrigation. Certain
vegetable crops like reddish, cauliflower, spinach etc were found to give better yield in this particular sewage water.

KEYWORDS: Sewage, irrigated. accumulation, heavy metal

Influence of Chloride Ion on the Corrosion Inhibition Efficiency of the ATMP - Zn 2+ System
C. Thangavelu, P. Patric Raymond, S. Rajendran and M. Sundaravadivelu…………………………………………….402

ABSTRACT:
Corrosion rates of carbon steel immersed in various concentrations of Cl- (100 ppm and 150 ppm) have been
evaluated by weight loss method in the absence and presence of Amino (trimethylene phosphonic acid) ATMP and
Zn2+. It is found that ATMP alone is corrosive at 100 ppm Cl- but at 150 ppm Cl- it shows some inhibition efficiency
(IE) due to deposition of Cl- on metal surface. However interestingly, ATMP shows very good IE in the presence of
Zn2+ at all concentrations of Cl-. A synergistic effect is noticed between ATMP and Zn2+. The protective film has
been analysed by surface analysis techniques and a suitable mechanism of corrosion inhibition is proposed.

KEYWORDS: Carbon steel, corrosion inhibition, chloride environment, phosphonic acid

Analysis of Midazolam in Small Volumes of Plasma Using High Performance Liquid Chromatography and
UV-Detection Method: Pharmacokinetics of Midazolam in Rats
Swapnil J. Dengle, Shriram M. Pathak, Chandra Mohan, Arumugam Karthik, Prashant Musmade, Krishnamurthy
Bhat and Nayanabhirama Udupa……………………………………………………………………………………………...406

ABSTRACT:
This research work aims to exploit the high selectivity and sensitivity of UV detector to develop and validate a high
performance liquid chromatography (HPLC) method having very small sampling volume, much better mass-
sensitive detection limit and lower operating cost for the determination of midazolam, known to have low oral
bioavailability, in rat plasma. The chromatographic separation was achieved using a Vydac C18 monomeric (250 ×
4. 6 mm inner diameter × 5-µm particle size) column with mobile phase comprising of acetonitrile and potassium
dihydrogen phosphate buffer (50:50 v/v), delivered isocratically at a flow rate of 1. 0 ml min-1. Diazepam was used
as an internal standard (I. S.). The chromatographic peak-area ratio, based on UV absorbency at 245 nm, was used
for quantitative analysis. The statistical evaluation of the method was examined and the method was found to be
precise and accurate with a linearity range of 5–3000 ng ml-1 (r > 0. 9980). The intra-day and inter-day precision
studies showed good reproducibility with coefficients of variation (C. V.) less than 4. 70%. The developed method is
simpler and more sensitive than previously reported methods. The analytical sensitivity and accuracy of this assay
were adequate for characterization of midazolam in rat plasma and the assay has been applied successfully to the
in vivo pharmacokinetic study of midazolam in rats. After midazolam (5 mg kg-1) was given orally, the maximum
concentration (Cmax) and the area under curve (AUC) were 120 ± 35. 38 ng ml-1 and 446. 52 ± 49. 04 ng h ml-1,
respectively. The oral bioavailability, F (%), was approximately 24. 75 ± 2. 72%. The developed method holds
upper hand over other methods reported in literature so far in terms of both, a small sample volume (200 µl), short
analysis time (12. 5 min). Our laboratory is actually involved in a study to investigate the drug-drug interaction
studies using oral midazolam as one of the cytochrome P450 (CYP3A) marker compounds in the rat model. The
established method provides a reliable bioanalytical methodology to carry out midazolam pharmacokinetics in rat
plasma. The small sample volume required makes it possible to study the full pharmacokinetic profile in individual
small animals, like the rat.

KEYWORDS: Midazolam, Rat Plasma, HPLC, Validation, Pharmacokinetics

Simultaneous Estimation of Cefixime and Ofloxacin by Derivative Spectroscopy Method
S. A. Shah, M. P. Vaghela, B. P. Marolia and K. L. Daxina. ……………………………………………………………...415

ABSTRACT:
Accurate, precise, rapid and economical method was developed for the estimation of Cefixime and Ofloxacin in
tablet dosage form. The first order derivative spectroscopy wavelengths selected for quantitation were 312. 0 nm for
Cefixime (zero cross for Ofloxacin) and 358. 2 nm for Ofloxacin (zero cross for Cefixime). In this method linearity
for detector response was observed in the concentration range of 5-40 g/ml for both Cefixime and Ofloxacin. The
proposed method was successfully applied for the simultaneous determination of both drugs in commercial tablet
preparation. The results of the analysis have been validated statistically and by recovery studies.

KEYWORDS: Cefixime; Ofloxacin; Derivative spectroscopy.

Interference Study on Artificial Sweeteners in Forensic Toxicological Screening by TLC

Mohd Idris, S.K. Shukla and T.R. Baggi……….……………………………………………………………………………..419

ABSTRACT:
A study was carried out to asses the possible interference of artificial sweeteners (Saccharin, sucralose, aspartame
and cyclamate) while screening for drugs and pesticides in stomach content, urine and tissues by TLC for forensic
toxicological purposes. Even though these sweeteners were extractable in acidic drugs extract and pesticide extract
but they did not interfere in the analysis of drugs and pesticides. Therefore the screening methods usually used in
forensic toxicological analysis for drugs and pesticides can be applied as such without any modification as the
artificial sweeteners were not found to interfere.

KEYWORDS: Artificial Sweeteners; Interference; Drugs; Pesticides; Forensic Toxicological Analysis

Synthesis and Biological Evaluation of 1-Naphthyl and 4-Biphenyl Derivatives of 2, 4, 5-Trisubstituted-1H-

Imidazoles as Antibacterial and Antifungal Agents.
S.D. Sawant, R.N. Patil and A.A. Baravkar…………………………………………………………………………………..423

ABSTRACT:
In current study, 2,4,5-trisubstituted-1H-imidazoles have been synthesized by starting from acid chloride preparation
of various aromatic acetic acids (Ar’) such as 1-naphthyl acetic acid and 4-biphenyl acetic acid, which are used as
such for the Friedel–Craft acylation (FCA) using various substituted aromatic nucleus (1a-b) (Ar) such as anisole,
thioanisole etc and anhydrous aluminium trichloride to get various ethanone derivatives (2c-d). Methylsulfanyl
group is converted into methylsulfonyl by refluxing former with glacial acetic acid and hydrogen peroxide to get
ethanone derivatives containing methylsulfonyl moiety (2e-f). These ethanone derivatives (2a-f) were subjected to
microwave irradiation for 90 secs to obtain diketones or ethanediones (3a-f). Ethanediones, in presence of acetic
acid, ammonium acetate and benzaldehyde offered targeted compounds (4a-f). The structural elucidation of
synthesized compounds was done using IR as well as 1H NMR spectroscopy and biological screening for
antibacterial action using E. coli and S. aureus and antifungal action using C. albicans and C. fumigatus was done
using cup plate agar diffusion method.

KEYWORDS: 1H-imidazole, Microwave irradiation, Antibacterial, Antifungal..

Studies on Ethanol Production from the Fruit Waste Using Ultrasound Assisted Fermentation
Mahesh S. Patil and Shrikant R. Kulkarni…………….……………………………………………………………………...429

ABSTRACT:
Production of ethanol from the fruit waste using Saccharomyces cerevisiae yeast has been investigated in ultrasound
bath. The effect of temperature, PH on ethanol production was studied and optimized. The Saccharomyces cerevisiae
yeast was found to yield maximum ethanol production to the extent of 7 %V under identical conditions.
Due to sonication, fermentation was achieved within short period of time. It was found that intra particle diffusion
resistance has been overcome due to sonication.

KEYWORDS: Ultrasound, Fermentation; Ethanol; Fruit waste; Saccharomyces cerevisiae

RP-HPLC Method for the Estimation of Atorvastatin Calcium in Bulk and Pharmaceutical Formulations
P. Nagaraju, B. Sridhar, P. Jitendra Kumar, U. Upendra rao, K. Hanumantha Rao and P.N.V. Gopal……………434

ABSTRACT:
The present work describes a simple reverse phase HPLC method for the estimation of Atorvastatin calcium in bulk
and pharmaceutical formulations. The estimation was carried out on phenomenex C18 (250 × 4.6 mm, 5µ) column
using a mobile phase containing of Acetonitrile: Ortho-phosphoric acid (0.1%): Tetrahydrofuran (48:0.04:52). The
eluent was monitored at 244 nm. The results have been validated statistically and recovery studies confirmed the
accuracy of proposed method.

KEYWORDS: HPLC, Validation, Atorvastatin calcium and Pharmaceutical formulation.

Development and Validation of Stability Indicating HPTLC Method for Determination of Trandolapril as
Bulk Drug
Sejal P. Gandhi, Mohit G. Dewani, Tejas C. Borole and Mrinalini C. Damle…………………………………………..437

ABSTRACT:
Trandolapril is a drug in current clinical practice as antihypertensive. It modulates the renin-angiotensin-aldosterone
system that plays a major part in regulating blood pressure. The present study describes degradation of Trandolapril
under different ICH prescribed stress conditions (hydrolysis, oxidation, dry heat, wet heat and photolysis) and
establishment of a stability-indicating HPTLC assay method. Though a separate peak for the products of degradation
was not obtained, the peak purity of the drug was observed. For HPTLC Silica Gel 60 F254 plate and mobile phase
consisting of ethyl methyl ketone : acetic acid (8 : 0.25) was used to achieve separation and quantitation was done
at 220 nm. The method was found to be simple, specific, precise, and stability indicating.

KEYWORDS: Trandolapril, Stress degradation, Validation, Stability indicating method.

Synthesis of Indophenazino Fused Azacarbazole Derivatives of Biological Interest

Veena Yadav and Nishant Yadav………..……………………………………………………………………………………..441

ABSTRACT:
Application of the Japp-Klingemann reaction on N-substituted-(3-hydroxymethylidine)-piperidin-4-one 6(a-d) with
4-indophenazine diazonium chloride (5) and 5-indophenazine diazonium chloride (9) yielded the corresponding 3-
(4-indophenazinyl)-hydrazone of N-substituted piperidin-4-ones 7(a-d) and 3-(5-indophenazinyl)-hydrazone of N-
substituted piperidin-4-ones 10(a-d) respectively. Fischer indolization of 7(a-d) and 10(a-d) hydrazones with Kent’s
reagent (4:1 mixture of acetic acid:HCl) afforded N-substituted-2,3-dihydro-14H-azacarbazolo(2,3-b)-pyrazino(2,3-
b)-11H-indole-1-ones 8(a-d) and N-substituted-2,3-dihydro-14H-azacarbazolo(2,3-b)-6H-pyrrolo (3,2-b)-
quinoxaline-1-ones 11(a-d) in moderate to good yield. All azacarbazole derivatives 8(a-d) and 11(a-d) were
characterized on the basis of their microanalysis, IR, 1H NMR and MS spectral data.

KEYWORDS: Indophenazine, Azacarbazole, Japp-Klingemann reaction, Fischer indole synthesis.

Terminalia chebula Retz. Stem Bark Extract: A Potent Natural Antioxidant

Jiby Elias, Rajesh M.G., Anish N.P., Manu M.S. and Iwin C.V………..………………………………………………….445

ABSTRACT:
In vitro antioxidant activities and preliminary phytochemical profiling of the methanol extract of the stem bark of
Terminalia chebula Retz.(METC) of Combretaceae family were investigated. Total reducing power of the extract
increased with increasing concentration which indicated that the plant has inherent antioxidant potential. The extract
at a concentration of 500µg/ml showed maximum activity of 2, 2-diphenyl- 2- picryl-hydrazyl (DPPH) (85.72%)
followed by nitric oxide (82.28%), superoxide (79.12%) and hydroxyl (77.28%) radicals. The IC50 values of DPPH,
nitric oxide, superoxide and hydroxyl radicals were 72µg/ml, 73µg/ml, 69µg/ml and 80µg/ml respectively. METC
had 28.6mg phenols per gram. METC showed the presence of phytoconstituents such as alkaloids, terpenoids,
saponins, quinines, anthroquinones, tannins, carbohydrates, volatile oils, and phenolics. However, glycoside,
coumarins, reducing sugars and resins were absent. Thin layer chromatogram showed two spots (Rf: 0.41, 0.56)
under visible light and six spots (Rf: 0.41, 0.49, 0.56, 0.62, 0.71) on exposure to Iodine vapour. The findings suggest
that the methanol extract of T. chebula possesses significant free radical scavenging activities in different in vitro
models and could be a potent source of natural antioxidants.

KEYWORDS: Antioxidant activity, reducing power, DPPH, phenol

In Vitro Anti Oxidant Study of Ethanolic Extract of Coldenia procumbens Linn

Beena P., Purnima S. and Kokilavani R…………………………………………………………………………………….450

ABSTRACT:
An investigation has been carried out to evaluate the in vitro antioxidant activity of ethanolic extract of Coldenia
procumbens Linn by Diphenyl-1-picryl hydrazyl method (DPPH) and Nitric oxide radical scavenging inhibition
activity method. Coldenia procumbens Linn has been widely used for a number of medicinal purposes especially in
Siddha medicine. However, the information available on the pharmacological activity of the plant is very limited.
Hence, it was proposed to carry out a preliminary in vitro analysis of the anti oxidant activity of the plant, which
gave promising results. The standards used were ascorbic acid and rutin. This is the first report of the antioxidant
activity of the plant.

KEYWORDS: Coldenia procumbens Linn, DPPH method, Nitric oxide radical scavenging inhibition activity
method.

Nutritional Potentials of Rhynchophorus phoenicis (Raphia palm weevil): Implications for Food Security
A. J.Chinweuba, I. E. Otuokere, M.C. Opara and G.U. Okafor……..…………………………………………………….452

ABSTRACT:
Proximate and chemical analysis were carried out on the Early Larva (EL) and Late Larva (LL) stages of Raphia
palm weevil (Rhynchophorus Phoenicis) to ascertain its nutrition potentials. The Late Larva stage had the highest
protein content of 10.50% while 9.10% was recorded for early larva stage. All other essential classes of food and
amino acids were detected in varying amounts. The values derived for macro elements such as calcium, potassium
and iron were (0.28 ± 0.01mg/100g), (455.00 ± 21.00mg/100g) and (6.50 ± 0.40mg/100g) respectively for Early
Larva stage; (0.27 ± 0.01mg/100g), (457.50 ± 10.61mg/100g) and (6.00 ± 1.10mg/100g) respectively for Late Larva
stage. The results of the mineral contents showed that nutritive contents of Phynchophorus phoenicis at LL stage are
higher than EL stage. The study attests that both stages of the insect larva could form a base for food security by
providing nutritious food to meet people dietary needs for active and healthy life.

KEYWORDS: Food security, Phynchophorus phoenicis, malnutrition, macro elements.

Synthesis and Antimicrobial Activity of Mannich Bases of 1-Isonicotinoylpyrazolidine-3, 5-Dione

Sudhir Bharadwaj, Bharat Parashar, Dimple K. Rathore and V.K. Sharma……….…………………………………...455

ABSTRACT:
1-isonicotinoylpyrazolidine-3, 5-dione (1) has been synthesized by the condensation of isonicotinohydrazide, diethyl
malonate and a catalytic amount of glacial acetic acid. A number of 1- isonicotinoylpyrazolidine-3, 5-dione
derivatives have been synthesized by the reaction of (1) with various primary as well as secondary amines in
the presence of formaldehyde. The reactions have been carried out following conventional procedure and also under
microwave irradiation. The microwave-assisted reactions are rapid, safe, high yielding and superior to conventional
methods. The structures of all the products are characterized by micro analytical data and spectroscopic techniques.
All the synthesized products are screened for their antibacterial activity against E. coli, P. aeriginosa, B. subtillis S.
aureus and C. albicans, A. niger.

KEYWORDS: 1-Isonicotinoylpyrazolidine-3, 5-dione, isonicotinohydrazide, diethyl malonate, conventional

method, formaldehyde, and mannich bases.
Comparative In vivo Evaluation of Propranolol hydrochloride following Oral and Transdermal
administration in Rabbits
V. Sai Kishore, T. E. Gopala Krishna Murthy and C. Mayuren……..…………………………………………………….461

ABSTRACT:
Membrane-moderated transdermal systems of Propranolol hydrochloride were prepared by incorporating the drug
reservoir within a shallow compartment moulded from a drug-impermeable backing membrane and 2% w/v
cellulose acetate rate-controlling membrane casted with ethyl acetate-methanol (8:2) employing dibutyl phthalate
(40% w/w of dry polymer) as plasticizer. The pharmacodynamic and pharmacokinetic performance of Propranolol
hydrochloride following transdermal administration was compared with that of oral administration. This study was
carried out in a randomized cross-over design in male New Zealand albino rabbits. The estimation of Propranolol
hydrochloride in plasma was carried out by LC-MS/MS method. The parameters such as maximum plasma
concentration (Cmax), time for peak plasma concentration (tmax), mean residence time (MRT) and area under curve
(AUC0 - ) were significantly (P< 0.001) differed following transdermal administration compared to oral
administration. The terminal elimination half life of transdermally delivered of Propranolol hydrochloride was found
to similar that of oral administration. The relative bioavailability of Propranolol hydrochloride was increased about
six fold after transdermal administration as compared to oral delivery. This may be due to the avoidance of first pass
effect of Propranolol hydrochloride. In agreement with pharmacokinetic data, maximum ß -blockade was obtained at
1 h after oral administration and decreased by 80% after 6 h. In the case of transdermal administration, a steady state
ß-blockade.was observed after 12.0 h and was prolonged over a period of 24 h. It was concluded that the relative
rate of extensive first pass metabolism was significantly reduced in transdermal administration, resulted in increased
relative bioavailability and reduced frequency of administration.

Evaluation of Citrillus vulgaris (Watermelon) Seed Oil As a Source of Alternative Energy to Diesel Oil
A.J. Chinweuba, I.E. Otuokere, M.C. Opara and G.U. Okafor…………………………………………………………..466

ABSTRACT:
Diesel engines represent most widely used machines in agriculture. The exhaust gases from the combustion of fossil
fuels in the engines pollute the environment. Watermelon seed (Citrillus vulgaris) oil was evaluated for its physical
and chemical properties as fuel for diesel engines. Oil was extracted from watermelon seed by soxhlet method. The
oil yield was 20% and the oil was comparatively analyzed for fuel properties: relative density, refractive index,
viscosity, water content, calorific value, gross calorific value ash content and burning characteristics. Trace metal
and IR spectra analysis were also determined. Results showed that the watermelon seed oil could be utilized as
substitute for diesel oil.

KEYWORDS: Diesel oil, Citrillus vulgaris, alternative, seed oil, fuel properties

Kinetics and Mechanism of Micelle-Catalysed Oxidation of DL-Alanine and Glycine by Chloromine-T

Farhat Hasan Khan and Mahboob Alam……………………………………………………………………………………468

ABSTRACT:
The kinetics of oxidation of DL-alanine by chloramine-T(CAT) in the absence of any surfactant has been studied
and compared with the kinetics parameters observed in the presence of anionic micelles of sodium dodecyl sulfate
(SDS) and cationic micelles of cetyl pyridinium chloride (CPC). The observed rate law in respect of [alanine] and
[oxidant] is given as:
d[CAT]
/
− = k [alanine] [CAT]
dt
/
Where k is a complex function of hydrogen ion concentration as well as surfactant concentration. In the presence
of CPC, the kinetic features of decarboxylation of DL-alanine are different from those observed in the case of
glycine.

KEYWORDS: Kinetics, oxidation, micelle catalysis, chloramine-T, decarboxylation of amino acids

Study on Ground Water Quality of Greater Visakhapatnam City, Andhra Pradesh from July, 2007 to June,
2008.
G.Srinivas Rao and G.Nageswara Rao……………………………………………………………………………………….481

ABSTRACT:
Water samples were collected from 14 open wells, 34 bore wells and two reservoirs to study the ground water
quality of Greater Visakhapatnam city. The samples were analyzed for the parameters like Temperature, pH,
Conductivity, Total dissolved solids, Dissolved Oxygen, Hardness, Calcium, Magnesium, Nitrate, Sodium,
Potassium, Chloride and Alkalinity. Low ionic concentrations in ground waters far (7-14 km distance) from the sea
coast were observed which are within the permissible limits of WHO and ISI standards. Ground waters close to the
sea coast i.e. one to two kilometers distance (60 to 150 feet depth) have high values of Conductivity, Total
dissolved solids, Hardness, Chloride, Calcium, Magnesium, Sodium and Potassium which are not in permissible
limits.

KEYWORDS: Ground water quality, Visakhapatnam, salt water.

Manganese (II, III, IV) Complexes of N-(2-Hydroxysalicyliden-1-Yl) Methyleneben- Zoylhydrazide; Synthesis

and Spectral Studies
Nirmal K. Kar……….…………………………………………………………………………………………………………....491

ABSTRACT:
Reaction of H2L [N-(2-hydroxysalicyliden-1-yl)methylenebenzoylhydrazide] with manganese(II) acetate
tetrahydrate and manganese(III) acetate dihydrate in methanol followed by addition of methanolic KOH results in
[Mn(L)2] and [Mn(L)(OH)(H2O)]. Further, complexes of the composition [Mn(L)(A)][where A = pyridine(py), 2-
picoline(2-pic), 3-picoline(3-pic) and 4-picoline(4-pic)] were synthesized from the reaction of H2L,
Mn(OAc)2.4H2O, KOH and pyridine bases. The structures of the complexes were confirmed on the basis of
elemental analysis, molar conductivity, magnetic moment, FT-IR, UV-Visible and ESR spectra. The molar
conductance values in DMF (N,N-dimethylformamide) suggest non-electrolytic nature of the complexes. Electronic
spectral studies suggest 6-coordinate and 4-coordinate metal ions in these complexes. IR spectra reveal that H2L
coordinates in enol-form in its complexes.

KEYWORDS: Manganese (II,III,IV) complexes, N-(2-hydroxysalicyliden-1-yl)methyleneben- zoylhydrazide,

pyridine bases

Stability Indicating HPLC Method for Simultaneous Determination of Repaglinide and Metformin
Hydrochloride in Pharmaceutical Dosage Form
Deepa R. Patel, Laxmanbhai J. Patel and Madhabhai M. Patel…………………………………………………………..500

ABSTRACT:
A simple, specific and accurate stability-indicating reversed phase high performance liquid chromatographic method
was developed for the simultaneous determination of Repaglinide and Metformin hydrochloride. An isocratic RP-
HPLC was achieved on younglin HPLC system using Varian C18 (250 4.6 mm i.d, 5 m particle size) column
with the mobile phase containing mixture of acetonitrile: 10mM ammonium acetate(pH 3.0, adjusted with
phosphoric acid) (70 : 30, v/v). The flow rate was 1.0ml/min and the eluent was monitored at 230nm. The retention
times of Repaglinide and Metformin hydrochloride were found to be 3.1 min and 5.58 min, respectively. Linearity
was established for Repaglinide and Metformin hydrochloride in the range of 0.5-3 µg/ml and 200-1200 µg/ml,
respectively. The percentage recoveries of Repaglinide and Metformin hydrochloride were found to be in the range
of 99.87%±0.7 and 99.89%±0.15 respectively. Both the drugs were subjected to acid, alkali, oxidation, and dry heat
degradation. The degradation studies indicated, Repaglinide and Metformin hydrochloride showed degradation in
acid, alkaline, H 2 O 2, and in dry heat condition. The degradation products of Repaglinide and Metformin
hydrochloride were well resolved from the pure drug with significant differences in their retention time values. This
method can be successfully employed for simultaneous quantitative analysis of Repaglinide and Metformin
hydrochloride in bulk drugs and formulations.

KEYWORDS: Repaglinide, Metformin hydrochloride, Stability indicating method, HPLC

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