scholarly journals Validated HPTLC Method for Quantification of Luteolin and Apigenin inPremna mucronataRoxb., Verbenaceae

2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Nayan G. Patel ◽  
Kalpana G. Patel ◽  
Kirti V. Patel ◽  
Tejal R. Gandhi
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
Methanolic Extract ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Reflection Mode ◽  
Limit Of Quantitation ◽  
Hptlc Method

A simple, rapid, and precise high-performance thin-layer chromatographic method was developed for quantitative estimation of luteolin and apigenin inPremna mucronataRoxb., family Verbenaceae. Separation was performed on silica gel 60 F254HPTLC plates using toluene : ethyl acetate : formic acid (6 : 4 : 0.3) as mobile phase for elution of markers from extract. The determination was carried out in fluorescence mode using densitometric absorbance-reflection mode at 366 nm for both luteolin and apigenin. The methanolic extract ofPremna mucronatawas found to contain 10.2 mg/g % luteolin and 0.165 mg/g % of apigenin. The method was validated in terms of linearity, LOD and LOQ, accuracy, precision, and specificity. The calibration curve was found to be linear between 200 and 1000 ng/band for luteolin and 50 and 250 ng/band for apigenin. For luteolin and apigenin, the limit of detection was found to be 42.6 ng/band and 7.97 ng/band while the limit of quantitation was found to be 129.08 ng/band and 24.155 ng/band, respectively. This developed validated method is capable of quantifying and resolving luteolin and apigenin and can be applicable for routine analysis of extract and plant as a whole.

Development and Validation of a Stability-Indicating HPTLC Method for the Estimation of Eszopiclone in Pharmaceutical Dosage Forms

2021 ◽  
Vol 11 (3) ◽  
pp. 219-223
Author(s):  
Vidhya K. Bhusari ◽  
Sunil R. Dhaneshwar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Stress Degradation ◽  
Bulk Drug ◽  
Hptlc Method

Objective: A simple, sensitive, selective, precise repeatable and stability-indicating high-performance thin layer chromatographic method was developed and validated for Eszopiclone in bulk drug and in formulation. Method: Silica gel 60 F-254, TLC precoated aluminium plates was used as the stationary phase for analyzing Eszopiclone and its degradation products, using mobile phase consisting toluene: ethyl acetate: methanol (6: 4: 2 v/v/v). Result: This mobile phase gave compact spots for Eszopiclone with Rf value of 0.52 ± 0.02. Eszopiclone was exposed to hydrolysis, oxidation, neutral and photolytic conditions for conducting stress degradation study. The peak of Eszopiclone and the degradation product was well resolved from each other with a significantly different Rf value. Densitometric estimation of Eszopiclone was performed at 304nm. A good linear plot was obtained in the concentration range of 150-300ng/spot. The method was validated for precision, accuracy (recovery) and robustness study. The limit of detection (LOD) and limit of quantitation (LOQ) was found to be 130ng/spot and 150ng/spot, respectively. Conclusion: The developed HPTLC method can separate Eszopiclone from its degradation products, hence stability studies can be performed using this method.

scholarly journals Quantitative Analysis of Phenobarbital in Dosage Form by Thin-Layer Chromatography Combined with Densitometry

2006 ◽  
Vol 89 (4) ◽  
pp. 995-998 ◽  
Author(s):  
Magdalena Wójciak-Kosior ◽  
Agnieszka Skalska ◽  
Grażyna Matysik ◽  
Magdalena Kryska
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Low Cost ◽  
Sensitivity Limit ◽  
Layer Chromatography ◽  
Hptlc Method

Abstract In this paper, a high-performance thin-layer chromatography (HPTLC) method combined with densitometry has been described. Chromatography was performed on silica gel Si 60F254 plates using dichloromethaneethyl acetateformic acid (9.5 + 0.5 + 0.1, v/v) mobile phase. This method has been successfully applied for the determination of phenobarbital in pharmaceuticals. Obtained results were comparable with traditionally used column high-performance liquid chromatography (HPLC) methods. For the proposed procedure, linearity (r > 0.999), sensitivity (limit of detection 0.4 g/spot), recovery (97.8102.1%), and repeatability were found to be satisfactory. The HPTLC-densitometry method has many advantages, such as simplicity, reasonable sensitivity, rapidity, and low cost, and it can be successfully used in routine quality control of multidrug preparations containing barbiturates.

Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

2019 ◽  
Vol 15 (3) ◽  
pp. 273-279
Author(s):  
Shweta G. Rangari ◽  
Nishikant A. Raut ◽  
Pradip W. Dhore
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Analysis Data ◽  
Peak Height ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

DEVELOPMENT OF HPTLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND ORNIDAZOLE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 36-43
Author(s):  
N. R Dighade ◽  
◽  
M. D Shende ◽  
A. V Kasture
Keyword(s):  
Quality Control ◽  
High Resolution ◽  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Routine Quality Control

A simple and accurate high performance thin layer chromatographic (HPLTC) method has been developed and validated as per ICH guidelines for estimations of Ciprofloxacin (CP) and Ornidazole (ORN) in combined dosage form. The mobile phase was acetonitrile: toluene: water and triethylamine (5.5:1.8:1.5:1.6 V/V) was found to be best which gave high resolution with Rf 0.16 and 0.84 for ciprofloxacin and ornidazole respectively. The linearity of ciprofloxacin and ornidazole was found to be in the range of 0.4 to 0.8 µg/mL and 0.4 to 0.8 µg/mL, respectively. The coefficient of correlation (r2 ) was found to be greater than 0.989 for both the components by this method. The tablet analyses result (n = 5) were found to be > 100.84 % by HPTLC for both the components. The proposed method was found to be simple, accurate and suitable for routine quality control of marketed formulations containing these drugs.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

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 SIMPLE ANALYTICAL METHOD FOR THE SIMULTANEOUS ESTIMATION OF HYDROCHLOROTHIAZIDE AND CANDESARTAN BY RP-HPLC

2017 ◽  
Vol 9 (6) ◽  
pp. 34
Author(s):  
Madhavi K. ◽  
Navamani M. ◽  
Prasanthi C.
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Pharmaceutical Industries

Objective: To develop a simple, rapid, economic, accurate and precise reverse phase-high performance liquid chromatographic (RP-HPLC) method for the determination of hydrochlorothiazide and candesartan in the pharmaceutical dosage form and to validate as per international conference on harmonization (ICH) guidelines.Methods: The chromatographic separation was performed on Silanol BDS C18 column (250 x 4.6 mm, 5 μm), a mobile phase consisting of water (pH adjusted to 2.8 with orthophosphoric acid): acetonitrile (30:70 % v/v), with a flow rate 1 ml/min and the detection wavelength of 210 nm using photodiode array (PDA) detector.Results: The developed method resulted in elution of hydrochlorothiazide at 2.28 min and candesartan at 4.28 min. The calibration curves were linear (r2=0.999) in the concentration range of 6.25-18.75 μg/ml and 8-24 μg/ml for hydrochlorothiazide and candesartan respectively. The percentage recoveries were found to be 99.78-100.39 for hydrochlorothiazide and 99.87-100.64 for candesartan. The limit of detection (LOD) was found to be 0.410 μg/ml and 0.699 μg/ml for hydrochlorothiazide and candesartan respectively. The limit of quantitation (LOQ) was found to be 1.367 μg/ml and 2.330 μg/ml for hydrochlorothiazide and candesartan respectively.Conclusion: A simple, economic, accurate, precise, linear and rapid RP-HPLC method was developed for simultaneous quantitative estimation of hydrochlorothiazide and candesartan in bulk and pharmaceutical formulation and the method was validated as per ICH guidelines. Hence, the method holds good for the routine analysis of hydrochlorothiazide and candesartan in various pharmaceutical industries as well as in academics.

Development and validation of a HPLC-UV method for the simultaneous detection and quantification of paclitaxel and sulforaphane in lipid based self-microemulsifying formulation

2019 ◽  
Vol 57 (10) ◽  
pp. 931-938 ◽  
Author(s):  
Mohammad M Kamal ◽  
Sami Nazzal
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Simultaneous Detection ◽  
Reversed Phase ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Simultaneous Delivery ◽  
Detection And Quantification

Abstract Paclitaxel (PTX) and sulforaphane (SFN) are known anticancer molecules. Their activity was found to be potentiated when tested concurrently. Only recently, however, a novel SFN enabled PTX self-microemulsifying formulation (SMEDDS) was developed for their simultaneous delivery. This necessitated the development of an analytical method for the simultaneous detection and quantitation of PTX and SFN. In this study, a simple and sensitive isocratic high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method was developed and validated per International Conference on Harmonization guidelines to satisfy this objective. Its application was demonstrated when quantifying the amount of PTX and SFN released from the SMEDDS in various dissolution media. The separation of the analytes was performed with the aid of a reversed phase C18 column at ambient temperature using a 60:40 mixture of acetonitrile and KH2PO4 buffer (pH 5.0) as the mobile phase. PTX and SFN peaks were detected at 202 nm with high resolution without interference from excipients. This method showed linearity within 2.5–100 μg/mL range with r2 &gt; 0.999. The limit of detection and lower limit of quantitation were 0.1638 and 0.4964 μg/mL for PTX and 0.4419 and 1.3389 μg/mL for SFN, respectively. A total of 98–101% of the injected samples was recovered with RSD of 0.06–0.68% indicating the suitability of the method for the simultaneous detection and quantitation of the molecules in dissolution media.

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.

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