scholarly journals Stability-Indicating High-Performance Thin-Layer Chromatographic Method for Quantitative Estimation of Emtricitabine in Bulk Drug and Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Atul S. Rathore ◽  
Lohidasan Sathiyanarayanan ◽  
Kakasaheb R. Mahadik
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Bulk Drug

A simple, sensitive, precise, specific and stability indicating high-performance thin-layer chromatographic (HPTLC) method for the determination of emtricitabine both in bulk drug and pharmaceutical dosage form was developed and validated. The method employed aluminium plates precoated with silica gel G60 F254 as the stationary phase. The solvent system consisted of toluene : ethyl acetate : methanol (2 : 8 : 1, v/v/v). This solvent system was found to give compact spots for emtricitabine with value . Densitometric analysis of emtricitabine was carried out in the absorbance mode at 284 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 30–110 ng spot−1. The method was validated for precision, limit of detection (LOD), limit of quantitation (LOQ), robustness, accuracy and specificity. Emtricitabine was subjected to acid and alkali hydrolysis, oxidation, neutral hydrolysis, photodegradation and dry heat treatment. Also the degraded products peaks were well resolved from the pure drug with significantly different values. Statistical analysis proved that the method is repeatable and specific for the estimation of the said drug. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

scholarly journals Development and Validation of Stability-Indicating HPTLC Determination of Tamsulosin in Bulk and Pharmaceutical Dosage Form

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
S. B. Bari ◽  
A. R. Bakhshi ◽  
P. S. Jain ◽  
S. J. Surana
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Mean Value ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A simple, economic, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis of tamsulosin hydrochloride, both as a bulk drug and in formulations, was developed and validated according to ICH guidelines. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase while the solvent system consisted of toluene  :  methanol  :  triethylamine (3.5  :  1.2  :  0.2 v/v). The system was found to give compact spot for drug ( value of ). Densitometric analysis of tamsulosin was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship, with respect to peak area in the concentration range 400–2400 ng per spot. The mean value ± SD of slope and intercept were and with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantitation were 20.49 and 62.10 ng per spot, respectively. Tamsulosin was subjected to hydrolysis, oxidation, and thermal degradation which indicate the drug is susceptible to hydrolysis, oxidation, and heat. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of tamsulosin.

STABILITY INDICATING HPTLC METHOD FOR THE ESTIMATION OF TICAGRELOR IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (10) ◽  
pp. 34-39
Author(s):  
◽  
Elakkiya L Shunmuganathan ◽  
F. A Mehta ◽  
U. K. Chhalotiya
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Hptlc Method

A simple, sensitive, and precise high-performance thin-layer chromatographic method has been developed for the estimation of Ticagrelor in pharmaceutical dosage form. The method employed Thin-layer chromatography (TLC) aluminum plates precoated with silica gel 60 F254 as the stationary phase, while the solvent system was found to be toluene: ethyl acetate: acetic acid (5:4:1V/V/V). The Rf value was observed to be 0.33± 0.008. The spot was densitometrically analyzed in absorbance mode at 305 nm. The method was linear in the range of 50-250 ng/ band for ticagrelor. The limit of detection for ticagrelor was found to be 0.826 ng/ band. The limit of quantification for ticagrelor was found to be 2.64 ng/band. Ticagrelor stock solution was subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photo degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their Rf values. Stressed samples were assayed using developed HPTLC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of ticagrelor in its formulation.

scholarly journals STABILITY-INDICATING HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF FORMOTEROL FUMARATE DIHYDRATE AND FLUTICASONE PROPIONATE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 149-155
Author(s):  
RAJASHI B PHARATE ◽  
SUNEELA S DHANESHWAR
Keyword(s):  
Fluticasone Propionate ◽  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug ◽  
Formoterol Fumarate

Objective: The objective of the present work was to develop validated stability-indicating high-performance thin-layer chromatographic method for simultaneous estimation of formoterol fumarate dihydrate (FFD) and fluticasone propionate (FP) in bulk drug and pharmaceutical dosage form. Methods: Pre-coated silica gel aluminum plates 60 F-254 were used as stationary phase. The mixture of toluene:ethyl acetate:formic acid (98%) (6:4:0.1; v/v/v) was used as a mobile phase. The densitometric quantification was carried out at 233 nm. The method was validated according to the ICH guidelines. The specificity and stability indicating the capability of the method were proven though degradation studies. Both drugs were subjected to acid (0.1N HCl) and base (0.1N NaOH) hydrolysis, oxidation (3% v/v H2O2), photolytic, and neutral degradation conditions. Results: The selected mobile phase resolved peaks of FFD and FP with Rf values 0.27±0.10 and 0.64±0.10, respectively. Determination coefficients of calibration curves were found to be 0.998 and 0.999 in the range of 1–3.5 μg/spot and 10–60 μg/spot for FFD and FP with an accuracy of 99.09% for FFD and 99.20% for FP. The degradation products of FFD and FP were resolved from the pure drug with significant differences in their retention factor values. Conclusion: The developed method is simple, accurate and can be successfully applied for quantification of FFD and FP in bulk drug and pharmaceutical dosage form, contributing to improve the quality control and assure the therapeutic efficacy.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

scholarly journals Development and Validation of Stability-Indicating Reverse Phase-High Performance Liquid Chromatography Method for Simultaneous Determination of Atenolol and Nifedipine in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 219-223
Author(s):  
Ansari Yaasir Ahmed ◽  
Qazi Shoeb ◽  
Umme Rumana ◽  
Patel Afroza ◽  
Pathan Vahid Tajkhan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Limit Of Quantitation

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.

Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC Method

2019 ◽  
Vol 16 (1) ◽  
pp. 104-112
Author(s):  
Dharmendra Jayantibhai Prajapati ◽  
Usmangani Khalilurraheman Chhalotiya ◽  
Minesh Dahyabhai Prajapati ◽  
Jalpa Upendrabhai Patel ◽  
Jaineel Vinodrai Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Synthetic Mixture ◽  
Cancer Drug ◽  
Limit Of Quantification ◽  
Stability Indicating

Objective: An impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of Enzalutamide in bulk and synthetic mixture. Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 &amp;#177; 0. 005 and the densitometric analysis was carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture.<P&gt;

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