Asian Journal of Research in Chemistry

R. K. Nanda ¹, Pradeep B. Yadav ¹, A. A. Kulkarni ¹

Affiliations
1 Padmashri Dr.D.Y. Patil Institute of Pharmaceutical Sciences and Research, Sant Tukaram Nagar, Pimpri, Pune-411018, Maharashtra, IN

Abstract

A high-performance thin layer chromatography (HPTLC) method for Atazanavir Sulfate (ATV) and Ritonavir (RTV) was developed in the present work. The mobile phase selected was Ethyl acetate: Toluene: methanol (7.5: 2: 0.5 v/v/v) with UV detection at 234 nm. The standard solution ranging from 1000-7000ng/band was applied for ATV and standard solution ranging from 500-3500ng/band was applied for RTV. Linearity was observed in this concentration range on precoated silica gel 60 F₂₅₄ TLC plate in the form of bands with 100 μl sample syringe using automatic sample applicator LINOMAT V. After development, plate was immediately dried and was observed under UV chamber. The well resolved bands of drugs were scanned with Camag TLC scanner III densitometer controlled by WINCAT's software version 4. Retention factor for ATV and RTV were found to be 0.76 ± 0.95 and 0.54 ± 1.43 respectively. Drugs were subjected to oxidation, acid hydrolysis, base hydrolysis and sun light to apply stress condition for degradation studies. Results of analysis were validated statistically and by recovery studies.

Keywords

Atazanavir Sulfate, Ritonavir, and HPTLC.

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R. K. Nanda ¹, S. E. Potawale ¹, V. V. Bhagwat ¹, S. C. Hamane ¹, R. S. Deshmukh ²

Affiliations
1 D.Y.Patil Pratishthan’s Padmashree Dr. D.Y.Patil Institute of Pharmaceutical, Sciences and Research, Pimpri, Pune-411018, IN
2 Sinhgad College of Pharmacy, Vadgaon, Pune-411041, IN

Abstract

A simple, precise, accurate and rapid HPLC method has been developed, and validated for the determination of Aspirin, Atorvastatin Calcium simultaneously, in combined dosage form. Acetonitrile: 0.02 M Phosphate buffer with pH 6.1 (50%:50% v/v) is used as the mobile phase, pH adjusted with Sodium Hydroxide (1% aqueous). Mobile phase was delivered at the flow rate of 1.0 ml/min., 239 nm is the detection wavelength for this study. The applicability of the method for simultaneous determination of Aspirin, Atorvastatin Calcium was verified by the determination of these compounds in marketed capsules. Results of the analysis were validated statistically, and by recovery studies. Linearity for Aspirin And Atorvastatin Calcium was in the range of 5-35 μg/ml and 1-7 μg/ml, respectively and reproducibility was found to be satisfactory. The % assay (Mean±S.D.) was found to be 99.33±0.501 and 101.4±0.18 for Aspirin and Atorvastatin Calcium respectively. The recovery and RSD values are within the limits given in ICH guide lines. Method development indicates the suitability of proposed method for the routine determination of these compounds in capsule dosage form. The proposed method can be successfully used to determine the drug contents of marketed formulation.

Keywords

RP-HPLC, Validation, Aspirin, Atorvastatin.

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R. K. Nanda ¹, V. V. Bhagwat ¹, S. E. Potawale ¹, S. C. Hamane ¹

Affiliations
1 Dr. D.Y.Patil Institute of Pharmaceutical Sciences and Research, Pimpri, Pune-411018, IN

Abstract

A new simple high performance thin layer chromatographic (HPTLC) method for simultaneous determination of Cefixime and Potassium Clavulanate combined tablet dosage form has been developed and validated. The separation was carried out on Merck aluminum plates precoated with silica gel 60 F₂₅₄, using Acetone: Water: Acetic acid 8:0.8:1.2 (v/v/v) as mobile phase. The separated spots were stained with Iodine vapors and scanned at 410 nm. The retention factor for Cefixime and Potassium Clavulanate were found to be 0.23±0.01 and 0.68±0.01. The method was validated with respect to linearity, accuracy, precision, robustness, in accordance with ICH guidelines. The calibration curve was found to be linear over a range of 0.5-3.0 μg per spot for Cefixime and 0.310-1.870 μg per spot for Potassium Clavulanate. The method has been successfully applied for the analysis of drugs in pharmaceutical formulation. The % assay (Mean±S.D.) was found to be 100.29±0.9933 for Cefixime and 100.95±1.005 for Potassium Clavulanate.

Keywords

Cefixime, Potassium Clavulanate, HPTLC, Tablet Dosage Form.

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R. K. Nanda ¹, S. E. Potawale ¹, V. V. Bhagwat ¹, S. C. Hamane ¹, R. S. Deshmukh ²

Affiliations
1 Dr. D. Y. Patil Institute of Pharmaceutical Sciences and Research, Pimpri, Pune-411018, IN
2 Sinhgad College of Pharmacy, Vadgaon, Pune-411041, IN

Abstract

A simple, precise and economical procedure for the simultaneous estimation of Aspirin and Atorvastatin Calcium in capsule formulation has been developed. The first method employs simultaneous equations (Method I) which involve absorbance measurement at 225.5 nm (λ max of Aspirin) and 246.0 (λ max of Atorvastatin Calcium). Second method involves absorbance ratio (Method II), which uses the ratio of absorbances measured at two selected wavelengths, one at isoabsorptive point (232.5 nm) and other being the max of one of the two compounds. Third method involves measurement of area under curve (AUC). For this method wavelength ranges were chosen between 223.5-227.5 nm and 244-248 nm for Aspirin and Atorvastatin Calcium respectively. Results of analysis for methods were tested and validated for various parameters according to ICH guidelines, hence can be adopted for the routine analysis of Aspirin and Atorvastatin Calcium in tablet dosage form.

Keywords

Aspirin, Atorvastatin Calcium, Simultaneous Equation Method, Absorbance Ratio Method, Area Under Curve Method.

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A. A. Kulkarni ¹, S. R. Doshi ¹, R. K. Nanda ¹, N. R. Chatterjee ²

Affiliations
1 Dr. D.Y. Patil Institute of Pharmaceutical Sciences and Research, Pimpri, Pune-411018, Maharashtra, IN
2 Dr. D.Y. Patil College of Pharmacy, Akurdi, Pune-411044, Maharashtra, IN

Abstract

Synthon approach is a very useful analytical tool. It is an analytical approach to Organic Synthesis in which the target molecule is broken into fragments through a series of logical disconnection to get the best plausible and likely starting materials (ie. synthons or building blocks) for the target molecule. Synthesis is the real test of the organic medicinal chemist to use and control organic reactions. In each case the starting material is converted to some desired compound, the target molecule through some key intermediate. Actually, a number of synthetic routes can be written for a given target molecule. But in actual synthesis, generally that route is selected which is economical, safe, and easy to carry out and produces maximum yield in a short reaction time.

Keywords

Synthon Approach, Synthon, Disconnection Rules.

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R. K. Nanda ¹, J. Gaikwad ¹, A. Prakash ¹, V. K. Ghosh ¹, D. H. Nagore ¹

Affiliations
1 Dr. D. Y. Patil Institute of Pharmaceutical Sciences and Research, Pimpri, Pune, IN

Abstract

Two accurate and precise methods were developed for the estimation of Cefixime and Erdosteine in its pharmaceutical dosage form. First method is area under the curve method; the areas under the curve in the range of 294.5-284.5 nm (for CEF) and 240.0-230.0 nm (for ERD) were selected for the analysis. Second method is first order derivative spectroscopy by solving simultaneous equation, 309.0 nm (for CEF) and 227.5 nm (for ERD) were selected for the analysis. In both the methods linearity for detector response was observed in the concentration range of 10-50 μg/ml for both Cefixime and Erdosteine. The proposed methods were successfully applied for the simultaneous determination of both drugs in its pharmaceutical preparation. The results of the analysis have been validated statistically and by recovery studies.

Keywords

Cefixime, Erdosteine, Area Under the Curve Method, Derivative Spectroscopy.

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R. K. Nanda ¹, J. Gaikwad ¹, A. Prakash ¹

Affiliations
1 Dr. D. Y. Patil Institute of Pharmaceutical Sciences and Research, Pimpri, Pune, Maharashtra, IN

Abstract

Three simple, precise and economical UV methods have been developed for the estimation of Tamsulosin in pharmaceutical dosage form. Tamsulosin has the absorbance maxima at 281.0 nm (Method A), and in the first order derivative spectra, showed sharp peak at 234.5 nm (Method B). Method C applied was area under curve (AUC), in the wavelength range of 286.0-276.0 nm. Linearity for detector response was observed in the concentration range of 5-25 μg/ml for all three methods. The proposed methods were successfully applied for the simultaneous determination of Tamsulosin in commercial pharmaceutical preparation. The results of the capsule analysis were validated statistically and by recovery studies. It was found to be satisfactory.

Keywords

Tamsulosin, Absorbance Maxima, Derivative Spectroscopy, Area Under Curve.

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