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K. Rajendra Prasad ¹, S. Kathirvel ¹

Affiliations
1 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi road, Guntur. A.P., IN

Abstract

A simple, rapid, sensitive and precise high performance liquid chromatography (HPLC) method has been developed for the estimation of Mycophenolate mofetil in bulk and pharmaceutical dosage form. In this method RP-C18 column (250mmx4.6mm I.D and5μm particle size) with mobile phase consisting of acetonitrile and 0.02M phosphate buffer in the ratio of 50:50 v/v in isocratic mode was used. The detection wavelength is 230 nm and the flow rate is 1 ml/min. In the range of 10-60 μg/ml, the linearity of Mycophenolate mofetil shows a correlation coefficient of 0.999. The proposed method was validated by determining sensitivity, accuracy, precision and system suitability parameters. The mobile phase selected for the method is simple, fast, accurate and precise and hence can be applied for routine quality control analysis of Mycophenolate mofetil in bulk and its pharmaceutical dosage form. The method was fully validated according to ICH guidelines.

Keywords

Mycophenolate Mofetil, High Performance Liquid Chromatography, Validation.

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K. Rajendra Prasad ¹, S. Kathirvel ¹

Affiliations
1 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur-522002, Andhra Pradesh, IN

Abstract

A simple, sensitive and accurate spectrophotometric method has been developed for the estimation of mycophenolate mofetil in bulk and pharmaceutical formulation. The method is based on the formation of green colored chromogen with 3-methyl-2-benzothiazolinone-hydrazonehydrochloride reagent in the presence of 0.03M ferric chloride and obeys beer's law in the range of 2-10 μg/mL exhibiting the maximum absorbance at 659 nm. The limit of detection and quantification were found to be 0.87 μg/mL and 2.66 μg/ mL respectively. The calibration curve demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.999. The regression equation of the curve is Y=0.082x-0.019. The method is fully validated according to ICH guidelines.

Keywords

Mycophenolate Mofetil, 0.03m Ferric Chloride, 3-Methyl-2-Benzothiazolinone Hydrazonehydrochloride (MBTH) Reagent, Validation, ICH Guidelines.

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S. Kathirvel ¹, R. Raju ¹, B. Seethadevi ², A. Suneetha ³, K. Jyothisree ³

Affiliations
1 Department of Pharmaceutical Analysis, National College of Pharmacy, Manassery, Kozhikode, Kerala, 673602, IN
2 Department of Pharmacognosy, National College of Pharmacy, Manassery, Kozhikode, Kerala, 673602, IN
3 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi road, Guntur, A.P, 522002, IN

Abstract

The study is a proposition of the application of high performance liquid chromatography (HPLC) with a spectrophotometric UV range detector to analyse the chemical purity and assay of tetrabenazine in bulk drug and tablet formulation and also to apply the proposed method to determine the content uniformity according to USP specification. During computer assisted literature search only a few publications were found about tetrabenazine, so the ultimate objective of the present investigation was aimed to develop stability - indicating LC method and the development of the newer analytical method was achieved under optimised chromatographic conditions by using mobile phase composed of potassium phosphate buffer: acetonitrile in the ratio (40:60v /v). The seperation was achieved by using isocratic elution mode with a flow rate of 1.0 mL/min. The effluent was monitored on a UV detector at 284 nm. The retention time of tetrabenazine was found to be at 5.05min and the standard calibration curve was linear over a concentration range of 6.25-37.5 μg/mL with r value of 0.999. The LOD and LOQ were found to be 0.562 and 1.704 μg/mL respectively. The recovery studies were performed and the percentage recoveries were found to be in the range of 98.64-98.88 %. The drug was also subjected to acidic, basic, oxidative and photolytic degradation as per the ICH guidelines. The developed method allows to separate all degradation from tetrabenazine and to quantitate the tetrabenazine amount. As there is no official monograph in the pharmacopeias about tetrabenazine, the performed full validation procedure makes the method ready to use in routine analysis.

Keywords

Content Uniformity, ICH Guidelines, Tetrabenazine And USP Specification.

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T. Gopi Raju ¹, M. Gayatri Ramya ², A. Rajesh ³, S. Kathirvel ³, Sanjay Kumar Gupta ⁴

Affiliations
1 Department of Pharmaceutical Chemistry, Telangana University, Nizamabad – 503322, IN
2 Department of Pharmaceutics, Acharya Nagarjuna University, Nagarjuna Nagar- 522 510, IN
3 Department of Pharmaceutics and Pharmaceutical Analysis, Hindu College of Pharmacy, Guntur -522002, IN
4 Department of Pharmaceutics, Shadan College of Pharmacy, Hyderabad, Andhra Pradesh -500008, IN

Abstract

A simple, precise, accurate and new stability-indicating reversed-phase high-performance liquid chromatographic (RPHPLC) method was developed and validated as per International Conference on Harmonisation (ICH) of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines to determine efafirenz in tablet dosage form. The drug was successfully eluted at 6.264 min by mixture of ammonium dihydrogen phosphate buffer, acetonitrile and triethylamine (30:70:1) on C18 column (150 mm × 4.6 mm, 5 μm) at the flow of 1.5 ml/min. Drug content was determined in between 99.79% and 100.33% with standard deviation of 0.217. The validated RP-HPLC method may be successfully applied for assay, dissolution studies, bio-equivalence studies, as well as routine analysis in pharmaceutical industries.

Keywords

RP-HPLC, Efavirenz, ICH.

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K. Madhu Babu ¹, S. Kathirvel ²

Affiliations
1 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur, Andhra Pradesh – 522002, IN
2 Hindu College of Pharmacy, Amaravathi Road, Guntur, Andhra Pradesh - 522002, IN

Abstract

A simple, sensitive, accurate spectrophotometric method has been developed for the estimation of Tapentadol hydrochloride in bulk and pharmaceutical formulation. The method is based on the formation of blue colored chromogen with Folin-Ciocalteu reagent in the presence of NaOH and obeys beer's law in the range of 5 - 35μg/mL exhibiting the maximum absorbance at 763nm. The limit of detection and quantification were found to be 0.76#956;g/mL and 2.33#956;g/mL respectively. The calibration curve demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.9999. The Regression Equation of the curve was Y=0.0248x-0.0436. The method was fully validated according to ICH guidelines.

Keywords

Tapentadol Hydrochloride, Folin-Ciocalteu (FC) Reagent, NaOH, Validation, ICH Guidelines.

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S. Kathirvel ¹, A. Suneetha ²

Affiliations
1 Hindu College of Pharmacy, Amaravathi Road, Guntur-500 002, A.P, IN
2 Hindu College of Pharmacy, Amaravathi Road, Guntur, Andhra Pradesh-522002, IN

Abstract

A simple, rapid, sensitive and precise HPLC method has been developed for the estimation of risperidone in oral solution. In this method RP-C18 Phenominex Gemini column (250 mm x 4.6 mm i.d.,5μm particle size) with mobile phase consisting of 0.5% ammonium acetate buffer, acetonitrile and methanol in the ratio of 50:20:30 v/v/v in isocratic mode was used. The detection wavelength is 260 nm and the flow rate is 1.5 mL/min. In the range of 20-100μg/mL, the linearity of risperidone shows a correlation coefficient of 0.9999. The percentage recovery ranges from 98.95-101.50%. The proposed method was validated by determining sensitivity, accuracy, precision and linearity.

Keywords

Risperidone, HPLC, Oral Solution, Validation.

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S. Kathirvel ¹, S. V. Satyanarayana ², G. Devalarao ³

Affiliations
1 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur, A.P, IN
2 Department of Chemical Engineering, JNTU College of Engineering, Anantapur, A.P, IN
3 Department of Pharmaceutical Analysis, K.V.S.R Siddhartha College of Pharmaceutical Sciences, Vijayawada, A.P, IN

Abstract

The present work describes a simple, precise and accurate HPLC method for estimation of darifenacin hydrobomide in bulk and in tablet dosage form. The separation was achieved by using Waters Sunfire C₁₈(4.6 X 250 mm) 5μm particle size column. The mobile phase consisted of 0.02M potassium dihydrogen phosphate buffer pH 7 adjusted with triethylamine: acetonitrile: methanol in the ratio of 40:30:30(v/v/v). Detection was carried out at 280 nm. The retention time of darifenacin hydrobromide was found to be 4.2 min respectively. The Limit of detection and limit of Quantification was found to be 2.112 μg/mL and 6.400 μg/mL respectively. The accuracy and reliability of the proposed method was ascertained by evaluating various validation parameters like linearity (10-100 μg/mL), precision, accuracy and specificity according to ICH guidelines. The proposed method provides an accurate and precise quality control tool for routine analysis of darifenacin hydrobromide in bulk and in tablet dosage form.

Keywords

Darifenacin Hydrobromide, HPLC, Method Development, Validation.

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S. Kathirvel ¹, R. Raju ¹, K. K. Aneesha Fasla ¹, V. P. Shahana ¹

Affiliations
1 Department of Pharmaceutical Analysis, National College of Pharmacy, Manassery, Mukkam Post, Kozhikode, Kerala, IN

Abstract

This write-up provides a review on the various sample preparation techniques involved in the analysis of the food substances and food products. The awareness about food safety is highlighted. The sampling procedure involved in food analysis is discussed. A different sample preparation method including its advantages and disadvantages are addressed. The applicability of the all the methods involved in sample preparation techniques of food analysis is also touched upon.

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S. Kathirvel ¹, R. Raju ¹, B. Seethadevi ¹, A. Suneetha ², J. Pavani ²

Affiliations
1 Department of Pharmaceutical Analysis, National College of Pharmacy, Manassery, Mukkom Post, Kerala, IN
2 Department of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur, A.P, IN

Abstract

The objective of the current study was to develop a validated, specific and stability-indicating reversed phase HPLC method for the quantitative determination of posaconazole and its related substances in API (Active Pharmaceutical Ingredient). The determination was done for active pharmaceutical ingredient in the presence of degradation products, and its process-related impurities. The chromatographic separation was achieved on a waters HPLC system with PDA detector and the column employed for the present investigation was inertsil ODS-3V C18 (150×4.6 mm with 5 μ particle size) and empower2 software provided by waters was used throughout the experiment. The method employed a linear gradient elution and the detection wavelength was set at 225 nm (for intermediate A impurity) and 260 nm (for intermediate B, diastereomer, formyl and benzyl posaconazole impurity). The drug was subjected to stress conditions of hydrolysis (acid and base), oxidation, photolysis and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to show the stability-indicating power of the method. Significant degradation was observed during acid, oxidative, thermal and photo stress studies. In the developed HPLC method, the resolution between posaconazole and its process-related impurities was found to be greater than 2.0. Regression analysis shows an r value (correlation coefficient) of greater than 0.999 for posaconazole and it’s all the five impurities. The developed HPLC method was validated with respect to linearity, accuracy, precision and robustness.

Keywords

Degradation Products, Posaconazole, Process-Related Impurities, Regression Analysis.

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S. Kathirvel ¹, G. Devala Rao ², S. V. Satyanarayana ³

Affiliations
1 Dept. of Pharmaceutical Analysis, Hindu College of Pharmacy, Amaravathi Road, Guntur-2, A.P, IN
2 Dept. of Pharmaceutical Analysis, KVSR Siddhartha College of Pharmacy, Vijayawada-10, A.P, IN
3 Dept. of Chemical Engineering, JNTU College of Engineering, Anantapur-515002, A.P, IN

Abstract

A simple, sensitive and economical UV spectrophotometric method has been developed for the determination of Risperidone in bulk and tablet dosage forms. Risperidone is an anti-psychotic drug, which shows maximum absorbance at 238 nm in 0.1 N HCl. Beer’s law was obeyed in the concentration range of 5-30 μg/ml with correlation coefficient of 0.9999.The standard plot clearly showed a straight line passing through the origin. The results of analysis were validated statistically and by recovery studies and found to be satisfactory. The proposed method was extended to pharmaceutical formulations and there was no interference of additives and excipients.

Keywords

Risperidone, UV Spectrophotometric, Tablet Dosage Form.

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