International Journal of Pharmaceutical Chemistry and Analysis

59-64

Authors: Bulbul Purkait , Anup Sharma.

Arnica Montana extract, a natural limuloid contains about 59 ingredients out of which sesquiterpene lactones helenalin, and dihydrohelenalin, are considered significant medicinally active ingredients. Arnica Montana is commonly used in folk medicine, CAM, and Homeopathic drug as neurotropic, cardiotropic, Anti-inflammatory, Anti-bacterial, Anti-oxidant, Anti tumors, to control diabetes, etc. The plant is often misidentified with similar plants. Arnica Montana is now a protected endangered plant species. The commercially available crude ethanol extract and serial dilutions of Arnica Montana is studied for identification and characterization using Scanning Electron Microscope and FTIR. Keywords: Arnica Montana, Lactones, Scanning Electron Microscopy, Vibrational Spectroscopy, Serial Dilution.

74-83

Authors: Jagdish Kumar, Mymoona Akhtar, Chanda Ranjan, Gita Chawla

A series of 5-substituted phenyl-3-(thiophen-2-yl)-4, 5-dihydro-1, 2-oxazoles (2a-l) was synthesized by reacting appropriate chalcones of 2-acetyl thiophene with hydroxylamine hydrochloride in the presence of dry pyridine. The newly synthesized compounds were characterized by IR, 1HNMR, 13CNMR and mass spectral data. All the compounds were evaluated for their antidepressant and antianxiety activities in mice by forced swimming test and elevated plus maze method respectively. Test compounds and imipramine were administered intraperitoneally in antidepressant study at dose of 10 mg/kg. Similarly to study antianxiety activity, test compounds at the dose of 10 mg/kg and diazepam at the dose of 2 mg/kg were administered intraperitoneally. However, preliminary antidepressant screening of compounds (2a-l) revealed that none of the compounds showed antidepressant activity except for compound 2k which moderately (P<0.05) reduced the duration of immobility time. This compound was also tested in-vitro for its MAO inhibitory effect. Compound 2f showed highest antianxiety activity compared to diazepam and did not show neurotoxicity in rotarod test. The compounds were also studied for pharmacokinetic parameters and was observed that compound 2f displayed good ADME properties. Keywords: Thiophene, isoxazole, antianxiety and antidepressant.

97-101

Authors: P.S. Jain, N.K. Kale, K. M. Agrawal, N. G. Haswani, S.J. Surana

A HPTLC/Densitometric method has been developed for the determination of Guaifenesin (GFN) in bulk and pharmaceutical formulation. The estimation of drug was performed on HPTLC aluminium plates precoated with silica gel 60 RP-18 TLC F254 S using toluene: methanol: ethyl acetate: acetic acid (7:0.8:1.2:0.5 v/v/v/v) as mobile phase. The densitometric quantification for the drug was carried out at 274 nm. GFN obeyed linearity in concentration range 800 – 2800 ng/band with coefficient of correlation 0.999. The Rf for GFN was found to be 0.6 ± 0.02. The proposed method was applied for pharmaceutical formulation and % label claim for GFN was found to be 100.34  1.06. The method was validated for accuracy, precision and ruggedness. Accuracy of the method was checked by recovery studies at three different levels i.e. 80 %, 100 % and 120 %. The % recovery of GFN was found to be in the range of 99.48% - 100.68 %; the % RSD value was less than 2 indicates the accuracy of the method. The method was found to be precise as indicated by the inter-day, intra-day and repeatability analysis; showing % RSD less than 2. The results did not show any statistical difference between operators showing that developed method was rugged. GFN was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acid-base conditions, hydrolysis, oxidation, photo degradation except dry heat degradation. This indicates that the drug is susceptible to acid and base. The degraded product was well resolved from the pure drug with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for the identification and quantitative determination of GFN in bulk drug and pharmaceutical formulation. Keywords: Guaifenesin, high-performance thin-layer chromatography (HPTLC), validation,stability, degradation.

108-112

Authors: Umang Shah, Tarang Talaviya, Anuradha Gajjar

A simple, novel, sensitive and precise validated spectrophotometric method was developed for simultaneous determination of Mebendazole (MBZ) and Levamisole Hydrochloride (LVM) in its tablet formulation. 1% H2SO4 in methanol was selected as a common solvent for estimation of MBZ and LVM. For first order derivative method, estimation of MBZ was carried out at 307nm (ZCP of LVM) and of LVM at 232.6nm (ZCP of MBZ). The linearity was obtained in the concentration ranges of 2-6 μg/mL for MBZ and 3-9 μg/mL for LVM with correlation coefficient(r2) value greater than 0.995 . The % RSD value for intraday & interday precision were less than 2. The detection limit and quantification limit were found to be 0.44 μg/mL and 1.34 μg/mL for MBZ and 0.14 μg/mL and 0.42 μg/mL for LVM, respectively. All the validation parameters were performed as per the ICHQ2 (R1) guidelines. The recovery study was carried out, results were 98.82 – 101.93 % for MBZ and 100.05-101.42% for LVM. So, the developed method could be applied for the routine quality control analysis of MBZ and LVM in combined tablet formulation. Keywords: Mebendazole, Levamisole Hydrochloride, First Order Derivatives, ICH guideline, Validation

14-21

Authors: Neelima Dhingra1, T.R.Bhardwaj2

Introduction and positioning of the heteroatom in the parental steroid skeleton has significant effect on the activity profile of these compounds. A substantial amount of biologically relevant azasteroids have been reported as antifungals, antilipemic, neuromuscular blocking agents, local anaesthetics, antimicrobials, and GABA receptor antagonist. Recent work from our laboratory has described the synthesis and evaluation of 17-Oxo-17a-aza-D-homo-5-androsten-3β-yl ester derivatives as potential 5-alpha reductase inhibitors. The current study was undertaken to further investigate the cytotoxicity of the newly synthesized derivative using some more human cancer cell lines. Seven human cancer cell lines have been exposed to 1X 10-5m (single dose) of compounds (1-8), Finasteride, 5-fluorouracil, mitocycin 6 and, adriamycin were used as reference drugs for comparison. The cell growth was measured after 24h, using ELISA reader, after staining with sulforhodamine B dye (SRB), which binds to basic amino acid residues in the trichloroacetic acid (TCA) fixed cells. All the experiments were carried out in quadruplicate. The newly synthesized azasteroids derivatives displayed significant cytotoxicity against liver and neuroblastoma cell lines as compared to standard reference drugs. This together with, earlier reported antiproliferative activity against prostate cancer cell lines (DU-145) and 5-alpha reductase inhibitory activity, indicates that 17a-azasteroids seems to possess potential eliciting in vitro cytotoxicity. Results obtained from these studies shall be used as guidelines for further development of novel compounds to be used chemotherapeutic agents.

28-33

Authors: P. S. Jain*, A. P. Gorle, S. S. Patil, R. S. Chavan, P. R. Bari, S. J. Surana

A new simple, precise, accurate and selective RP-HPLC method has been developed and validated for estimation of salmeterol xinafoate in pharmaceutical formulation. The method was carried out on a Qualisil RP C-18 (250 mm x 4.6 mm, 5 μm) column with a mobile phase consisting of buffer: acetonitrile: methanol (45:25:30 v/v/v), pH adjusted to 6 with diammonium hydrogen orthophosphate and flow rate of 0.5 mL/min. Detection was carried out at 250 nm. The retention time for salmeterol xinafoate was found to be 7.41 min. The salmeterol xinafoate followed linearity in the concentration range of 1- 6 μg/mL (r2= 0.9984). The amount of the drug estimated by proposed method was found to be in good agreement with label claim. The developed method was validated for sensitivity, accuracy, precision, ruggedness and robustness. The LOD and LOQ were found to be 0.10 and 0.29 μg. Salmeterol xinafoate was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and thermal conditions. This indicates that the drug is susceptible to acid, base, oxidation and thermal conditions. The degraded product was well resolved from the pure drug with significantly different Retention Time. The proposed method can be used for routine analysis of salmeterol xinafoate in bulk drug and pharmaceutical formulation.

38-41

Authors: Neethu Mathew1,*, M. Sukumar2, T. K Ravi3, Arunkumar R4, Betty Carla5

Various N-[3-Chloro-2-(substituted)-4-oxazetidin-1-yl]-4-(1H-indol-3-yl) butanamide derivatives have been synthesized by the cyclo condensation of Schiff bases with tri ethyl amine and chloro acetyl chloride. The structures of the newly synthesized compounds have been established on the basis of their spectral data. All compounds were evaluated for α-amylase inhibitory activity. All compounds investigated exhibited significant activity, comparable to that of the standard used.

46-50

Authors: Sankalp Yadav1*, Gautam Rawal2

The world is facing the problem of substandard or spurious drugs. These substandard drugs have resulted in life threatening issues, financial loss of consumer and manufacturer and loss in trust on health system. The problem is graver in developing countries where these drugs are easily available to the people. There is an urgent need to address this issue and take measures to control the widespread availability and usage. Although, India has taken some preventive measures to fight against the problem of substandard/spurious drugs for protecting and promoting the public health but, still a lot needs to be done.

6-13

Authors: Amol. Y. Ghodke, Bhagwat. N. Poul, Mohini. B. Sorde.

A simple, specific, precise and accurate Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the quantitative estimation of Torsemide in Bulk and Pharmaceutical dosage form. The proposed RP-HPLC method was carried out on Zorbax C18 (250x4.6mm), 5μm column with mobile phase phosphate buffer and methanol (50:50) (v/v). The pH of phosphate buffer was adjusted by Ortho- phosphoric acid to 3.5. The flow rate was 1.3 mL/min and the detection wavelength was 288nm. The retention time of torsemide was found at 6.0±0.2min. The method was validated for specificity, precision, accuracy, linearity and robustness. The linearity range was 10-30 μg/mL and correlation coefficient (r2) was found to be 0.9980. The mean % recovery for Torsemide was found to be 99.80. The developed method could be employed for the routine analysis of Torsemide from different formulations and for the Torsemide calculations as well.

39-46

Authors: S. K. Gupta, Pankaj Baboo.

N-Phenyl anthranilic acid was prepared by Ullmann condensation of o-chlorobenzoic acid and aniline. The N-phenyl anthranilic acid was cyclized with polyphosphoric acid over a water bath at 100°C to form acridin-9(10H)-one. N10-Alkylated acridin-9-ones were synthesized in two series, in first series, N10-alkylation with 1-bromo-3-chloro propane and in second series with 1, 2-dichloroethane were done by using tetrabutyl ammonium bromide as phase transfer catalyst. Later both were derivatized by refluxing with different secondary amines in presence of potassium carbonate using anhydrous acetonitrile as solvent. The newly synthesized compounds were purified by column chromatography. The formation of title compounds confirmed by physical and spectral data. The synthesized compounds were subjected to microbiological screening.

58-64

Authors: Amol. Y. Ghodke, Bhagwat. N. Poul, Patil Bhagyashree R.

A simple, specific, precise and accurate Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the estimation of Diltiazem HCl (Diltiazem Hydrochloride) in Bulk and Pharmaceutical dosage form. The chromatographic determination was performed on isocretic High performance liquid chromatography system of Agilent model no.1220. The separation was conducted by using column of Zorbax [C8 (5µ, 4.6mm×250)] with mobile phase consisting of buffer and Acetonitrile in the ratio of (60:40). The mobile phase was delivered at the flow rate of 1.0ml/min. The eluent was monitored at wavelength 240 nm and found a sharp and symmetrical peak with retention time of 4.66min. The method was validated for linearity, accuracy, precision, specificity, robustness. Recovery of Diltiazem HCl was found to be in the range of 98%-102%. The method was found to be linear over the concentration range 50-150 µg/ml with coefficient correlation r2 = 0.995. After developing method and studying validation parameter to obtain result complying with USP monograph.