scholarly journals Development and Validation of UV Spectrophotometric Method for Quantitative Estimation of Clobetasol 17-Propionate

2016 ◽  
Vol 1 (1) ◽  
pp. 36 ◽  
Author(s):  
Neelam Devi ◽  
Sunil Kumar ◽  
Sunny Rajan ◽  
Jagbir Gegoria ◽  
Sheefali Mahant ◽  
...  

Clobetasol 17-propionate is used most potent topical glucocorticoid clinical effective in treatment of topical dermatitis, vitiligo and psoriasis. A rapid, simple, selective and precise UV- Visible Spectrophotometric method has been developed for the determination of Clobetasol 17-Propionate (CP) in bulk forms and dosage formulations. The spectrophotometric detection was carried out at an absorption maximum of 239 nm using ethanol as solvent. The method was validated for specificity, linearity, accuracy, precision, and robustness. The detector response for the CP was linear over the selected concentration range 2 to 40μg/ml with a correlation coefficient of 0.9999. The accuracy was between 99.1 and 101.4 %. The precision of 4μg/ml sample preparation three times in a day (intraday) was 0.1325%. The Limit of Detection (LOD) and Limit of Quantification (LOQ) are 0.84 and 2.55μg/ml, respectively. The recovery of CP was about 101.84%. The results demonstrated that the excipients in the commercial formulation did not interfere with the method and can be conveniently employed for daily routine quality control analysis of CP in bulk drug, marketed formulations.

Author(s):  
ANUJA SURYAWANSHI ◽  
AFAQUEANSARI ◽  
MALLINATH KALSHETTI

Objective: The present work is aimed to develop a simple, rapid, selective and economical UV spectrophotometric method for quantitative determination of Glipizideinbulk and pharmaceutical dosage form. Methods: In this method Dimethyl Form amide (DMF) was used as solvent, the absorption maxima was found to be275 nm in DMF. The developed method was validated for linearity, accuracy, precision, ruggedness, robustness, LOD and LOQ in accordance with the requirements of ICH guideline. Results: The linearity was found to be 10-60 µg/ml having linear equation y=0.017x-0.006 with correlation coefficient of 0.997. The% recovery was found to be in the range of 98.7-100%. The % RSD for intra-day and inter-day precision was found to be 0.569923 and 0.40169 respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be3.06 µg/ml and 9.27 µg/ml respectively. Conclusion: The developed method was validated as per ICH Q2(R1) guidelines. The novel method is applicable for the analysis of bulk drug in its pharmaceutical dosage form.


2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.


2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.


2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Neelkant Prasad ◽  
Roshan Issarani ◽  
Badri Prakash Nagori

A simple and sensitive ultraviolet spectrophotometric method for quantitative estimation of glipizide in presence of lipid turbidity is described to avoid false estimation due to diffraction by turbidity. UV detection was performed at 230 nm, 225 nm, and 235 nm, and the calibration curve was plotted between resultant of absorbance of [230 nm − (225 nm + 235 nm)/2] and concentration of analyte. The calibration curve was linear over the concentration range tested (1–20 μg/mL) with limit of detection of 0.27 μg/mL and limit of quantification of 0.82 μg/mL. Percent relative standard deviations and percent relative mean error, representing precision and accuracy, respectively, for clear as well as turbid solutions, were found to be within acceptable limits, that is, always less than 0.69 and 0.41, respectively, for clear solution and 0.65 and 0.47, respectively, for turbid solution. Conclusively, our method was successfully applied for the determination of glipizide in clear as well as turbid solutions, and it was found that the drug analyte in both types of solutions can be detected from the same calibration curve accurately and precisely and glipizide entrapped in the liposomes or in proliposomal matrix was not detected.


Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.


2008 ◽  
Vol 5 (4) ◽  
pp. 706-712 ◽  
Author(s):  
A. V. Sulebhavikar ◽  
U. D. Pawar ◽  
K. V. Mangoankar ◽  
N. D. Prabhu-Navelkar

A rapid and simple high performance thin layer chromatography (HPTLC) method with densitometry at λ=263 nm was developed and validated for simultaneous determination of lopinavir and ritonavir from pharmaceutical preparation. Separation was performed on aluminum-backed silica gel 60F254HPTLC plates as stationary phase and using a mobile phase comprising of toluene, ethyl acetate, methanol and glacial acetic acid, in the volume ratio of 7.0:2.0:0.5:0.5 (v/v) respectively. After development, plates were observed under UV light. The detector response was linear in the range of 6.67 to 20.00 µg/spot and 1.67 to 5.00 µg/spot for lopinavir and ritonavir respectively. The validated lowest limit of detection was 21.00 ng/spot and 5.10 ng/spot whereas lowest limit of quantification was 7.00 ng/spot and 21.00 ng/spot for lopinavir and ritonavir respectively. The percentage assay of lopinavir and ritonavir was found between 98.23 to 102.28% and 98.03 to 103.50% respectively. The described method has the advantage of being rapid and easy. Hence it can be applied for routine quality control analysis of lopinavir and ritonavir from pharmaceutical preparation and stability studies.


2018 ◽  
Vol 10 (1) ◽  
pp. 74 ◽  
Author(s):  
Ayya Rajendra Prasad ◽  
Bannaravuri Thireesha

Objective: To develop and validate a novel, specific, precise and simple UV-spectrophotometric method for the estimation of lornoxicam present in microsponges.Methods: UV-spectrophotometric determination was performed with Thermo Scientific Evolution 201 UV-Vis spectrophotometer using methanol as a medium. The spectrum of the standard solution was run from 200-400 nm range for the determination of absorption maximum (λ max). λ max of lornoxicam was found at 353 nm. The absorbance of standard solutions of 3, 6, 9, 12 and 15, µg/ml of drug solution was measured at an absorption maximum at 353 nm against the blank. Then a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 3.0-15.0 µg/ml with a correlation coefficient of 0.9995. The limit of detection (LOD) and limit of quantification (LOQ) for lornoxicam was found at 1.26 μg/ml and 3.82 μg/ml respectively. Accuracy was in between 99.21 and 99.60%. % RSD for repeatability, intraday precision and interday precision were found to be 0.473, in between 0.478 and 0.619 and in between 0.855 and 1.818 respectively. The proposed UV method is found to be robust.Conclusion: The proposed UV-Visible spectrophotometric method was validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable and simple for the estimation of lornoxicam present in microsponges.


2017 ◽  
Vol 6 (5) ◽  
pp. 196-199 ◽  
Author(s):  
Shahinaz Mohammed ◽  
Mohammed Adam ◽  
Shaza Shantier

In this study a simple, accurate and precise UV- spectrophotometric method was developed for the estimation of bisoprolol fumarate (BF) in bulk and tablet dosage form. The method was based on measurement of absorbance of BF aqueous solution at 271nm. Validation was conducted in accordance to ICH guidelines. The calibration curve was linear in the concentration range 5-25 µg/mL with correlation coefficient not less than 0.9986. The limit of detection and limit of quantification were 0.22 μg/ml and 0.66 μg/ml, respectively. Intraday and intermediate precision of the developed method were reflected by the low RSD% values (1.19 and 0.854, respectively). The recovery percentage was 105.0 ± 1.3%, n=3. The proposed method was applied for the assay of BF in three different brands


Author(s):  
Ankit Acharya ◽  
N.K. Satish ◽  
L. Manoj ◽  
Renukaradhya Chitti

The main objective of present study is to develop and validate a new, simple, precise and accurate RP-HPLC method for the determination of Darifenacin Hydrobromide (DFH) in bulk and pharmaceutical dosage forms. The separation and quantification of the drug was achieved on a RP C18 column (250×4.6mm, 5μm) using a mobile phase of acetonitrile: buffer (50:50), pH 3.0 ± 0.2 at a flow rate of 1 mL/min with detection of analyte at 287 nm. The separation was achieved with in 4.0 ± 0.3 min. The method showed good linearity in the range of 10-100 μg/mL. The intra and inter day RSD ranged from 0.20-0.58%. The recovery (mean ± SD) of low, medium and high concentrations were 98.50 ± 0.20, 100.27 ± 0.15 and 100.90 ± 0.09 respectively. The limit of detection and limit of quantification were 0.31 and 0.61 μg/mL, respectively. It can be concluded that the present method could be superior over the methods which were reported earlier. Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 36-44 


2021 ◽  
Vol 36 (2) ◽  
pp. 106-115
Author(s):  
Osama I. G. Khreit ◽  
Abdulsalam Elfowiris ◽  
Abdulrahman A. Aljali ◽  
Omukalthum Abduljalil

Acrylamide is a potential health hazardous compound occurring in baked and fried food as a result of excessive dry heating during the preparation and/or processing of foods. Exposure to a high level of acrylamide may cause cancer, neurotoxicity, and mutagenicity. In this study, an isocratic reversed-phase high-performance liquid chromatographic (HPLC) method using a C18 column was used for the determination of acrylamide in selected food. The mobile phase consisted of 0.1% formic acid in water: acetonitrile (98:02), and the flow rate was 1.0 mL min-1, elution was monitored at 200 nm. Validation in selected conditions showed that the chosen method is sensitive, selective, precise, and reproducible with a linear detector response for the determination of acrylamide. The limit of detection (LOD), and the limit of quantification (LOQ), were achieved at 0.41μg mL-1 and 1.25 μg mL-1respectively. The proposed method was also applied after validation to the most popular six brands of chips and French fries available in the Libyan market. Acrylamide was extracted by a simplified extraction method avoiding cleanup by solid-phase extraction (SPE), then analyzed by HPLC-UV. The highest level of acrylamide was found in one brand of chips with a concentration of 16.33 μg mL-1, whereas only one of the French fries products analyzed exhibited an acrylamide concentration of 10.26 μg mL-1.


Sign in / Sign up

Export Citation Format

Share Document