scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR STABILITY INDICATING HPTLC METHOD FOR ASSAY OF STIRIPENTOL IN BULK AND DOSAGE FORM

2021 ◽  
Vol 3 (4) ◽  
pp. 26-30
Author(s):  
Santosh Kumar Kashid ◽  
Amit Tapkir ◽  
Pravin Choudhari
Keyword(s):  
Room Temperature ◽  
Method Development ◽  
Limit Of Detection ◽  
Acidic Condition ◽  
Calibration Plot ◽  
Stability Indicating ◽  
Study Results ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Introduction: This work is concerned with the stability-indicating method development and validation of Stiripentol in a bulk drug and formulation by high-performance thin-layer chromatographic method (HPTLC). Materials and Methods:The pre-coated silica gel 60 F254 aluminum plate was selected as the stationary phase, and the solvent system consisted of Ethyl acetate: Dichloromethane: Toluene (2:2:6 v/v) used as developing solvents. Analysis of Stiripentol was carried out at 301 nm with Stiripentol being detected at an R(f) of 0.63. The developed method was validated for linearity, accuracy, precision, limit of detection (LoD), limit of quantitation (LoQ), robustness parameters, and stability are determined by force degradation study. Results and Discussion: The correlation coefficient of Stiripentol was 0.994 observed. The calibration plot was linear between 50–300 ng/band, respectively. The average percentage recovery of Stiripentol was found to be 100.25 %. Intra and inter-day precision measured as %RSD was less than 2%. Hence stability study of Stiripentol, it was found to degrade in acidic condition(8.52% - 0.1N HCL for 30 minutes at room temperature), alkali condition(7.47%- 0.1 N NaOH for 30min at room temperature), Hydrolytic condition(4.73%– dist. Water for 30min at room temperature), thermal condition(7.69%-40°C for 30min ), oxidative condition(7.55% - 3% H2O2 for 30min at room temperature) and photolytic UV condition(7.54% -24hr UV radiation) respectively. Stiripentol was unstable in acidic condition and stable in normal dist. Water hydrolytic condition. Conclusion: The proposed method was found to be very sensitive and accurate for the determination of Stiripentol in bulk and formulation.

Formulation, method development and validation of water soluble vitamins B1, B2 & B6 in bulk and tablet dosage form by HPTLC method

2018 ◽  
Vol 5 (1) ◽  
pp. 1-4
Author(s):  
Devi Velmurugan ◽  
Jambulingam Munusamy ◽  
Ananda Thangadurai Subramaniam ◽  
Anandkumar Karunakaran ◽  
Abdul Latiff MKM ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Water Soluble ◽  
Good Resolution ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Hptlc Method

In the present study we are reporting  dissolution, method development and validation of water soluble vitamins B1, B2 & B6 in bulk and tablet dosage form by HPTLC method. The method is based on separation of the three vitamins using HPTLC. Thin layer chromatographic plates coated with silica gel 60F254 as the stationary phase and acetonitrile:water (6:4 v/v) as mobile phase. The chromatographic analysis was carried out in the reflectance and absorbance mode at 280 nm. The method was validated with respect to linearity, accuracy and precision, limit of detection and limit of quantitation. It was then applied for analysis of vitamins B1, B2 & B6 in combined tablet dosage form. The above method developed was reproducible with good resolution and the results of analysis have been validated with correlation coefficient of 0.9990

scholarly journals Method Development and Validation for Determination of Voglibose in Tablet Formulation Using LC-MS/MS

2011 ◽  
Vol 8 (4) ◽  
pp. 1770-1783
Author(s):  
Mithlesh Rajput ◽  
Meenakshi Dahiya ◽  
Premlata Kumari ◽  
Kamini Kalra ◽  
Manjeet Aggarwal ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantitation ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Treatment Of Diabetes ◽  
Tablet Formulations ◽  
Development And Validation

Voglibose is a potent α glucosidase inhibitor, used for the treatment of diabetes mellitus. For quantitative determination of voglibose in pharmaceutical formulations of low doses, simple, sensitive, accurate and precise LC-MS/MS method using electrospray ionization in positive mode was developed and validated. The method was found linear in the concentration range of 25.0-1200 ηg/mL with a correlation coefficient of 0.9998. The limit of detection (LOD) of the method was found to be 1.5 ηg/mL and limit of quantitation (LOQ) was achieved at 3.0 ηg/mL. The recoveries of voglibose from spiked samples at different concentration levels were found in the range of 98-102%. The proposed method was found suitable for quantitation of voglibose and for the determination of uniformity of content of the dosage units of the tablet formulations.

scholarly journals Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

2018 ◽  
Vol 5 (1) ◽  
pp. 1-11 ◽  
Author(s):  
Oman Zuas ◽  
Harry Budiman ◽  
Dieni Mansur ◽  
Muhammad Rizky Mulyana
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Analytical Data ◽  
Sample Treatment ◽  
Gaseous Products ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Abstract This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD) method for the measurement of the gaseous products of hydrodeoxygenation (HDO). The method validation parameters include selectivity, precision (repeatability and reproducibility), accuracy, linearity, limit of detection (LoD), limit of quantitation (LoQ), and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO) from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD) less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

scholarly journals A novel high performance liquid chromatography method development and validation of fluconazole by ezchrom software

2020 ◽  
Vol 11 (2) ◽  
pp. 2399-2409
Author(s):  
Vikrant Verma ◽  
Manish Pathak ◽  
Amit Kumar ◽  
Amit Kumar
Keyword(s):  
Standard Deviation ◽  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

The current research explains the development of a new method and its subsequent validation by a novel HPLC method in fluconazole tablets. Inertsil Octadecyl silica C18 column having dimensions of length 150 mm, diameter 4.6 mm, particle size 5 μm was exploited for the method development, and the mobile phase embodies buffer pH 4 and acetonitrile in the combo of 40:60. Wavelength exploited for the segregation was 289 nm. The volume of injection was preserved at 20 µl. The new developed method has been established to demonstrate linearity in the range of 10 to 30 µg /ml correspondingly. Average recovery established to be 101.571, 100.315, and 99.021, the standard deviation was established to be 0.93834, 0.986418, and 0.989741, and % R.S.D was established to be 0.92382, 0.98331, and 0.999526. The percentage recovery was established to be within prescribed restrictions. The limit of detection was established to be 0.0080. The limit of quantitation was established to be 0.0051. In assay studies, an average assay was found to be 95.966, and standard deviation and % RSD of the assay was found to be 0.6021  and  0.6274, respectively. The method was found to be specific as there was no intrusion from impurities and excipients. Extensive diversity of mobile phase combos was utilized for the research and flow rate preserved at 1.3 ml/min all through the process. After carefull and systemic investigation of various research articles and review articles, it is observed that H.P.L.C method development and validation of fluconazole has been done in various pharmaceutical dosage forms, but till now a smaller amount of work is executed on dosage forms of solid nature, and hence there is huge prospective for research to be done in this area for new methodology to be developed in pharmaceutical dosage form of solid nature by means of dissimilar mobile phase combos and different strategy adopted by use of chromatography software which avoids the problems and demerits associated with present methods

scholarly journals UPLC Method Development and Validation for the Determination of Chlophedianol Hydrochloride in Syrup Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 25-31
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Calibration Plot ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A specific, precise, accurate ultra pressure liquid chromatography (UPLC) method is developed for estimation of chlophedianol hydrochloride in bulk drug and syrup dosage form. The method employed with Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) in a gradient mode, with mobile phase of methanol and acetonitrile in the ratio of 65:35 %v/v. The flow rate was 0.1 ml/min and effluent was monitored at 254 nm. Retention time was found to be 1.130±0.005 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ)in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was good linear relationship between response and concentration in the range of 20-100 μg/ml respectively. The LOD and LOQ values were found to be 2.094(μg/ml)and 6.3466(μg/ml)respectively. No chromatographic interference from syrup excipients and degradants were found. The proposed method was successfully used for estimation of chlophedianol hydrochloride in syrup dosage form.

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