scholarly journals A Validated HPTLC Densitometric Method for The Quantitative Determination of Ubidecarenone in Bulk and in Capsule Formulation

2021 ◽  
Vol 3 (4) ◽  
pp. 197-207
Author(s):  
Anandakumar Karunakaran ◽  
Anjana Elampulakkadu ◽  
Ramesh Jayaprakash ◽  
Senthilkumar Raju ◽  
Meka Dharshini Lakshmiganesh
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Control Analysis ◽  
Phase Detection ◽  
Capsule Formulation ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Label Claim ◽  
Tlc Plates

A new, simple, precise, accurate and rapid high performance thin layer chromatographic method has been developed and validated for the estimation of ubidecarenone in bulk and in capsule formulation. The chromatographic separation was performed on aluminium TLC plates precoated with silica gel 60F254 as a stationary phase and methanol:water (7:3) as a mobile phase. Detection was performed densitometrically in the absorbance mode at 280nm for the evaluation of chromatograms. The system has given well sharp peak of ubidecarenone (Rf=0.51±0.02). The linearity of the method was established in the range of 1-6 ng/µL with correlation coefficient (r2) of 0.9995. The method was validated for precision, accuracy, robustness, ruggedness, LOD, and LOQ as per ICH guidelines. The limit of detection was found to be 0.0392 ng/µL, whereas the limit of quantitation was found to be 0.1189 ng/µL. The percentage label claim for ubidecarenone in the capsule formulation was found to be 99.96±0.4703. The accuracy of the method was confirmed by recovery studies. The percentage recovery was found to be in the range of 100.10-101.45% for ubidecarenone. The % RSD value was found to be less than 2. The low %RSD value indicates that there is no interference due to excipients used in the formulation. Hence, the developed method was found to be simple, precise, accurate, and rapid for the analysis of ubidecarenone in bulk and pharmaceutical formulation and it can be effectively applied for the quality control analysis of ubidecarenone in bulk and pharmaceutical formulation.

RP-HPLC METHOD FOR ESTIMATION OF LORNOXICAM IN TABLETS AND IN DISSOLUTION SAMPLES USING MASS SPECTROMETRIC COMPATIBLE BUFFERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Mass Spectrometric ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.

HPTLC Separation of a Hepatoprotective Combination in Pharmaceutical Formulation and Human Plasma

2020 ◽  
Vol 58 (5) ◽  
pp. 411-417
Author(s):  
Maimana A Magdy ◽  
Rehab M Abdelfatah
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Spiked Plasma ◽  
Significant Difference ◽  
Developing System

Abstract A binary mixture of Silymarin (SR) and Vitamin E (VE) acetate, of an antioxidant and a hepatoprotective effect, has been analyzed using a sensitive, selective and economic high performance thin layer chromatographic (HPTLC) method in their pure forms, pharmaceutical formulation and spiked human plasma. SR and VE were separated on 60F254 silica gel plates using hexane:acetone:formic acid (7:3:0.15, v/v/v) as a developing system with UV detection at 215 nm. The method was evaluated for linearity, accuracy, precision, selectivity, limit of detection (LOD) and limit of quantification (LOQ). SR and VE were detected in the linear range of 0.2–2.5 and 0.2–4.5 μg/band, respectively. Method validation was done as per ICH guidelines and acceptable results of accuracy of 99.86 ± 1.190 and 100.22 ± 1.609 for SR and VE, respectively were obtained. The method has been successfully applied for determination of the studied drugs in their pharmaceutical formulation without any interference from excipients, and in spiked plasma samples. Results obtained by the developed HPTLC-densitometric method were statistically compared to those obtained by the reported HPLC methods and no significant difference was found between them.

scholarly journals Development and Validation of UV-Spectrophotometric and HPLC Method determination of Dofetilide in Formulation

2020 ◽  
Vol 13 (2) ◽  
pp. 60-70
Author(s):  
Harsha Dhurve ◽  
Yasmini Parshuramkar ◽  
Milind Umekar ◽  
Krishna Gupta
Keyword(s):  
Detection Limit ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Label Claim ◽  
Photodiode Array ◽  
Development And Validation ◽  
Good Agreement

A new, simple, specific and economic UV Spectrophotometric method and HPLC method for the estimation of Dofetilide content in bulk and laboratory prepared mixture. UV spectrophotometric detection was carried out at absorption maxima (λmax) at 231nm using methanol as a solvent. The quantitation of drug was carried out using A1% 1cm at 231nm and Beer’s law was obeyed in the concentration range of 2.5-20 μg/ml, with correlation coefficient value less than 1.The chromatographic separation was carried on a C-18 (250 mm × 4.6 mm, 5μ) column using an isocratic mode with a mixture of Acetonitrile:Phosphate Buffer (pH-7) in the ratio of 55:45% v/v as a mobile phase. The flow rate was 1.5ml/min, temperature is maintained at ambient and detection was made at 231 nm using Photodiode array (PDA) detector. The developed method was validated according to ICH guidelines and different analytical parameters such as linearity, precision, accuracy, specificity, limit of detection, limit of quantitation were determined. The percent amount of drug estimated was nearly 100%, found to be a good agreement with label claim of prepared laboratory mixture. The proposed method was validated for its accuracy, precision, robustness, ruggedness, linearity, limit of detection, limit of quantitation and was found to be in range (% RSD<2.0 and SD <±2.0). Both methods were validated and found to be simple, sensitive, accurate, and precise. The results of the study and statistical data proved the applicability of the present method in routine analysis of Dofetilide in bulk as well as laboratory prepared mixture.

scholarly journals A Validated HPTLC Densitometric Method for Quantitative Determination of Zanamivir in Bulk and Pharmaceutical Formulation

2018 ◽  
Vol 9 (2) ◽  
pp. 115-120 ◽  
Author(s):  
Mohammed Al Bratty ◽  
Safaa Fathy Saleh ◽  
Hassan Ahmad Alhazmi ◽  
Sadique Akhtar Javed ◽  
Adel Mohammed Ahmed ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Antiviral Agent ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Tlc Plates ◽  
Pure Drug ◽  
Hptlc Method

The main purpose of the present study was to develop and validate a high performance thin layer chromatographic (HPTLC) method for quantitative determination of an antiviral agent, zanamivir in pure drug and diskhaler powder formulation. Chromatography was performed on aluminum TLC plates pre-coated with silica gel 60F254, employing a mixture of chloroform:methanol:ammonia (9.5:3.2:0.2,v:v:v) as mobile phase. The TLC scanner was operated in the absorbance mode at a wavelength of 230 nm for evaluation of chromatograms. The system has given well resolved peak of zanamivir (Rf = 0.56). The linearity of the method was established in the range of 20-300 ng/spot; correlation coefficient (r) was 0.9995. The low values of limit of detection and limit of quantification (12.4 and 37.5 ng/spot, respectively) have demonstrated the sensitivity of the developed method. The reported method was precise in both intra-day as well as inter-day analysis; % RSD of peak area was found to be less than 2%, and has an accuracy within 100 ± 2%. The developed method has a potential to quantify zanamivir from its diskhaler formulation without any interference from other components. The applicability of the method was demonstrated by excellent recovery of analyte (99.8%) from diskhaler formulation. The current analytical method can be applied for routine analysis of zanamivir in pure form and pharmaceutical formulation in quality control laboratories. 

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

Application of a Validated RP-HPLC Method in Solubility and Dissolution Testing for Simultaneous Estimation of Diacerein and Its Active Metabolite Rhein in Presence of Coformers in the Eutectic Tablet Formulation

2020 ◽  
Author(s):  
Rajeshri D Patel ◽  
Mihir K Raval ◽  
Trupesh M Pethani
Keyword(s):  
Active Metabolite ◽  
High Performance ◽  
Limit Of Detection ◽  
Oral Formulation ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Gradient System ◽  
Control Analysis ◽  
Chromatography Method ◽  
Limit Of Quantitation

Abstract The present study aimed to develop and validate a novel reversed-phase high-performance liquid chromatography method for simultaneous estimation of Diacerein (DIA) and Rhein (Rh, alkaline degradation product and active metabolite) in the presence of various coformers used to prepare eutectic oral formulation. Chromatographic separations were achieved on a Phenomenex Gemini C18 column (250 mm × 4.6 mm, 5 μm) placed in the thermostated column oven at 40°C. The mobile phase, comprising of acetonitrile and 10 mM ammonium acetate (pH 3.0), was eluted through the gradient system with 0.8 mL/min flow rate at 254 nm detection and analytical run time of 14 min. Additionally, the method was validated for specificity, linearity, precision, accuracy, selectivity, limit of quantitation, limit of detection and robustness as per International Conference on Harmonization guideline. The developed method was applied for the comparison of drug release profiles of pure DIA and from prepared eutectic formulations for the quantitation of DIA and Rh in the multicomponent adducts. The achieved method advocated their applicability in routine quality control analysis of DIA formulations without interference of degraded product and excipients.

ESTIMATION OF METFORMIN HYDROCHLORIDE AND TENELIGLIPTIN IN PHARMACEUTICAL FORMULATION BY HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHY

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 34-39
Author(s):  
V. B Patel ◽  
◽  
J. S. Patel ◽  
D. A Shah
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Retention Factor ◽  
Metformin Hydrochloride ◽  
Phase Detection ◽  
Chromatographic Separations ◽  
Ich Guidelines ◽  
Tlc Plates ◽  
Tablet Dosage ◽  
Layer Chromatography

A new, accurate and precise high performance thin layer chromatographic (HPTLC) method has been developed for simultaneous analysis of metformin hydrochloride and teneligliptin in tablet formulation. The chromatographic separations were achieved on TLC plates precoated with silica gel G60 F254 and the plates were developed with 0.5% ammonium acetate-n propanol-ammonia (4.5:5:0.5, v/v/v) as mobile phase. Detection and evaluation of chromatograms were performed densitometrically at 252 nm. The retention factor of metformin hydrochloride and teneligliptin was found to be 0.2 and 0.63, respectively. The method was found to be linear in the range of 100-1200 ng per spot and 200-2400 ng per spot for metformin and teneligliptin, respectively. The method was validated with respect to precision, accuracy, specificity and robustness as per ICH guidelines Q2 (R1) and the results were found to be within the acceptance criteria. The method was successfully applied for the analysis of drugs in combined tablet dosage form.

scholarly journals Estimation of Berberine in Ayurvedic Formulations Containing Berberis aristata

2008 ◽  
Vol 91 (5) ◽  
pp. 1149-1153 ◽  
Author(s):  
Kedar Kumar Rout ◽  
Subhalaxmi Pradhan ◽  
Sagar Kumar Mishra
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Calibration Plot ◽  
Methanolic Extracts ◽  
Limit Of Quantitation ◽  
Tlc Plates ◽  
Hptlc Method

Abstract A sensitive, simple, rapid, and efficient high-performance thin-layer chromatographic (HPTLC) method has been developed and validated for the analysis of berberine in marketed Ayurvedic formulations containing Berberis aristata DC for regulatory purposes. Chromatography of methanolic extracts of these formulations was performed on silica gel 60 F254 aluminum-backed TLC plates of 0.2 mm layer thickness. The plate was developed up to 66 mm with the ternary-mobile phase butanolacetic acidwater (8 + 1 + 1, v/v/v) at 33 5C with 5 min of tank saturation. The marker, berberine, was quantified at its maximum absorbance of 350 nm. The limit of detection and limit of quantitation values were found to be 5 and 10 ng/spot. The linear regression analysis data for the calibration plot showed a good linear relationship with correlation coefficient 0.9994 in the concentration range of 10 to 50 ng/spot for berberine with respect to peak area. The instrumental precision was found to be 0.49 coefficient of variation (CV), and repeatability of the method was 0.73 CV. Recovery values from 98.27 to 99.11 indicate excellent accuracy of the method. The developed HPTLC method is very accurate, precise, and cost-effective, and it has been successfully applied to the assay of marketed formulations containing B. aristata for determination of berberine.

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 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.

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