Asian Journal of Research in Chemistry

M. M. Maste ¹, A. N. Parate ², A. R. Bhat ¹

Affiliations
1 Department of Pharmaceutical Chemistry, KLEU’s College of Pharmacy, JNMC Campus, Nehrunagar, Belgaum-10, Karnataka, IN
2 Department of Pharmaceutical Analysis, Prin. K.M. Kundnani College of Pharmacy, Jote Joy Building, Cuffe Parade, Mumbai, IN

Abstract

A gradient LC method was developed for determination and quantitation of Sitagliptin in bulk drug and pharmaceutical formulations. The separation was accomplished on a symmetry reversed phase C18 column, 75 mm × 4.6mm I.D., 3.5μm column using mobile phase consist of acetonitrile and 0.03% formic acid at flow rate of 0.3ml/min. The eluents were monitored with a UV detector set at 268 nm as detection wavelength. The investigated validation elements showed the method has acceptable specificity, accuracy, linearity, precision, robustness. This method was found to be linear within range of 100 to 500 μg.ml^-1 (r=0.9999). The method could be of use for rapid and routine quality control analysis of Sitagliptin. Thus, the developed method can be used for process development as well as quality assurance of Sitagliptin in bulk drug and pharmaceutical formulations.

Keywords

Sitagliptin Phosphate, RP-HPLC, Validation, Liquid Chromatography, Quality Assurance.

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M. C. Kalekar ¹, A. R. Bhat ¹, V. R. Koli ¹

Affiliations
1 Department of Pharmaceutical Chemistry, K. L.E.U’s College of Pharmacy, Belgaum, IN

Abstract

Compound (3-oxo-3, 4-dihydro-2H-1, 4-benzothiazin-2-yl) acetic acid was synthesized by reacting o-Amino thiophenol and maleic anhydride. (3-oxo-3, 4-dihydro-2H-1, 4-benzothiazin-2-yl) acetate was prepared by Esterification of (3-oxo-3, 4-dihydro-2H-1, 4-benzothiazin-2-yl) acetic acid. Further eight Mannich bases were synthesized by using substituted Aromatic amines. The structures of synthesized compounds were confirmed on basis of IR, NMR and Mass Spectra. All synthesized compounds were screened for their antibacterial activity against strains viz. E. coli, E.fecalis, Klebshilla and S. aureus and antifungal activity against strains viz. C. albican and Aspergillus Niger. [4-({[4-( N-(5-methyl-4,5-dihydroisoxazol-3-yl)-aminosulfonyl) phenyl] amino} methyl)-3-oxo-3,4-dihydro- 2H-1,4-benzothiazin-2-yl]acetic acid, Ethyl[4-({[4-(N-(5-methyl-4,5-dihydro isoxazol-3-yl)-aminosulfonyl)phenyl] amino} methyl)-3-oxo-3,4-dihydro-2H-1,4-benzo thiazin-2-yl]acetate, [4-({[4-(N-pyridin-aminosulfonyl) phenyl] amino} methyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazin-2-yl]acetic acid and Ethyl [4-({[4-(N-pyridin-aminosulfonyl) phenyl]amino}methyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazin-2-yl]acetate have shown significant antibacterial and antifungal activity, while other derivatives shown moderate antibacterial and antifungal activity.

Keywords

1, 4 Benzothiazine, 1, 4 Benzothiazine Ester, Antibacterial, Antifungal.

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M. M. Maste ¹, A. N. Parate ², A. R. Bhat ¹

Affiliations
1 Department of Pharmaceutical Chemistry, KLEU’s College of Pharmacy, JNMC Campus, Nehrunagar, Belgaum-10, Karnataka, IN
2 Department of Pharmaceutical Analysis, Prin. K.M. Kundnani College of Pharmacy, Jote Joy Building, Cuffe Parade, Mumbai, IN

Abstract

A gradient LC method was developed for determination and quantitation of Sitagliptin in bulk drug and pharmaceutical formulations. The separation was accomplished on a symmetry reversed phase C18 column, 75 mm ×4.6mm I.D., 3.5μm column using mobile phase consist of acetonitrile and 0.03% formic acid at flow rate of 0.3ml/min. The eluents were monitored with a UV detector set at 268 nm as detection wavelength. The investigated validation elements showed the method has acceptable specificity, accuracy, linearity, precision, robustness. This method was found to be linear within range of 100 to 500 μg.ml^-1 (r=0.9999). The method could be of use for rapid and routine quality control analysis of Sitagliptin. Thus, the developed method can be used for process development as well as quality assurance of Sitagliptin in bulk drug and pharmaceutical formulations.

Keywords

Sitagliptin Phosphate, RP-HPLC, Validation, Liquid Chromatography, Quality Assurance.

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V. R. Lohar ¹, Mane Aruna ², Chavan jaykar ², M. S. Palled ¹, A. R. Bhat ¹

Affiliations
1 Department of Pharmaceutical Chemistry, KLEU’s College of Pharmacy, JNMC Campus, Nehrunagar, Belgaum-10, Karnataka, IN
2 Quality Assurance and Technical Services, Okasa Pharma Pvt. Ltd., Satara, Maharashtra, IN

Abstract

A simple, selective, rapid, precise and economical RP HPLC method has been developed for the determination of Paracetamol, Caffeine, Pseudoephedrine Hydrochloride, Dextromethorphan Hydrobromide and Loratadine in tablet formulation. The analysis was resolved by using a mobile phase (Sodium heptane sulphonate buffer solution and Acetonitrile in the ratio of 95:5) at a flow rate of 1ml/min on an gradient consisting of Shimadzu LC 2010 HPLC system on variable wavelength UV detector using, Inertsil ODS 3V (4.6 mm x 5 cm, 3 μm) column at a wavelength of 205 nm. The retention time were found to be Paracetamol (3.5min), Caffeine (5.5min), Pseudoephedrine HCl (8min), Dextromethorphan HBr (14min), Loratadine (15min). The percent recovery of Paracetamol, Caffeine, Pseudoephedrine Hydrochloride, Dextromethorphan Hydrobromide and Loratadine were found to be in between 98% to 102%. The developed method was simple, precise, accurate and reproducible and therefore suitable for routine analysis of drugs in tablet dosage form.

Keywords

Paracetamol, Caffeine, Pseudoephedrine HCl, Dextromethorphan HBr, Loratadine.

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M. M. Maste ¹, M. C. Kalekar ¹, N. Kadian ¹, A. R. Bhat ¹

Affiliations
1 Department of Pharmaceutical Chemistry, KLEU’s College of Pharmacy, Belgaum, IN

Abstract

Present work describes a precise, accurate and reproducible Reverse phase High Performance Liquid Chromatographic (RP-HPLC) method for simultaneous estimation of Ramipril and Amlodipine in tablet dosage form on Phenomenex C₁₈ column (245 mm × 4.5 mm, 5 μm, particle size) using acetonitrile: phosphate buffer, (60:40 v/v) as mobile phase at flow rate of 1.0 ml/min and the detection wavelength was 222 nm. The retention time for Ramipril and Amlodipine was found to be 3.41 and 6.10 min respectively. Proposed method was validated for precision, accuracy, linearity range, robustness and ruggedness.

Keywords

Amlodipine, Ramipril, RP-HPLC.

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M. Maste Meenaxi ¹, R. Ainapure ¹, P. B. Patil ¹, A. R. Bhat ¹

Affiliations
1 KLE University’s College of Pharmacy, JNMC Campus, Belgaum-590 010, Karnataka, IN

Abstract

The Nitro containing 5-oxo-[1,2,4,]triazole ring were synthesized by the nitration of compound (I) with nitric acid. Then acetic acid ethyl esters containing 5-oxo-[1,2,4,]triazole ring (II) were synthesized by the condensation of compound (I) with ethyl chloroacetate in basic media. The reaction of compound (II) with hydrazine hydrate led to formation of acid hydrazide (III). The treatment of compound(III) with different aromatic aldhydes resulted in the formation of arylidene hydrazide's as target compounds. The structure of the synthesized Compounds were evaluated by IR, ¹H NMR spectra and elemental method of analysis. All the synthesized compounds were screened for their antitubercular activity. Anti-tubercular activity was carried out by using middle brook 7H9 broth base (M198) medium against Mycobacterium tuberculosis of H37Rv Strain. Streptomycin was used as standard drug for comparison.

Keywords

5-Oxo-[1,2,4,]Triazole, Acid Hydrazide, Arylidene Hydrazides, Anti-Tubercular Activities, Mycobacterium tuberculosis.

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M. M. Maste ¹, P. Jeyarani ¹, M. C. Kalekar ¹, A. R. Bhat ¹

Affiliations
1 Department of Pharmaceutical Chemistry, K. L.E.U’s College of Pharmacy, Belgaum, IN

Abstract

The present research work was aimed to synthesize some benzimidazole acetic acid derivatives and also the derivatives associated with 1,2,4 triazolone and was investigated for their biological activities. A two different series of compounds were synthesized, 4-[(2-aryl methyl- 1H-benzimidazol-1-yl) acetyl] 5 nitro-2,4 -dihydro-3H-1,2,4 triazol- 3-one and 4-[(2-aryl methyl-1H-benzimidazol-1-yl)methyl] 5 nitro-2,4- dihydro-3H-1,2,4 triazol-3-one. The newly synthesized compounds have been characterized by their analytical and spectral (IR and ¹H NMR, C¹³ NMR, mass spectra) properties. All the compounds have been screened for their anti tubercular and antimicrobial activities by standard methods. Results of activities reveal that compound shown promising anti tubercular activity at both the concentration compared to standard drug streptomycin, and shown good antimicrobial activities.

Keywords

1,2,4 Triazolone, Benzimidazole, Anti Tubercular, Anti Bacterial , Antifungal Activity.

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K. Vaghela Gayatri ¹, S. B. Patil ², M. S. Palled ², A. R. Bhat ²

Affiliations
1 Fisher BioPharma Services (India) Pvt. Ltd, "PHARMEZ" SEZ, Plot No 22, Matoda, National Highway 8A, Ahmedabad-382213, Gujarat, IN
2 K.L.E.S’s College of Pharmacy, JNMC Campus, Belgaum-590010, Karnataka, IN

Abstract

Various derivatives of 4-thaizolidinones were synthesized by reacting Schiff bases with thioglycollic acid. These alcoholic groups were further oxidized to get the carboxylic acid derivatives. The compounds were purified using flash chromatography and were characterized by physical, chemical and elemental analysis. The compounds were screened for calcium antagonistic activity on albino rats by using Biopack data acquisition system. Some compounds showed comparable activity with standard drug Diltiazem.

Keywords

4-Thiazolidinones, Calcium Antagonist, Calcium Channel Blockers, Schiff Bases.

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