scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

A new simple RP-HPLC Method development, Validation and Forced degradation studies of Bilastine

2021 ◽  
pp. 183-187
Author(s):  
Khushbu K. Patel ◽  
Arati M. Patel ◽  
C. N. Patel
Keyword(s):  
Retention Time ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Hplc Method Development

A new simple, rapid, accurate and precise method for estimation of Bilastine in pharmaceutical dosage form by reverse phase liquid chromatography. The developed method employed mobile phase was Acetonitrile and Ammonium acetate pH 5.0 adjusted with glacial acetic acid with 85:15% v/v and flow rate 1.0ml/min. Method was developed using column C18 Water (150 × 4.6mm, 5µm) and detection wavelength was 215nm. The retention time was found to be 2.519 min. the proposed method was successfully applied to the determination of Bilastine in dosage form. High linearity of developed method was confirmed over concentration range of 25- 150 µg/ml and co-relation co-efficient is 0.996. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The recovery was in the range of 99 – 102% and limit of detection was found to be 0.45µg/ml and limit of quantification was found to be 1.20µg/ml. Bilastine was found to degrade under acid and oxidation conditions. There was no interference of excipient and degradation product in retention time so method was specific. Analytical parameter such as precision, accuracy, limit of detection, limit of quantification and robustness were determined according to international Conference on Harmonization (ICH) guidelines.

scholarly journals Method Development and Validation of Quantitative Estimation of Vilazodone Hydrochloride by UV and RP-HPLC

2020 ◽  
Vol 13 (4) ◽  
pp. 362-373
Author(s):  
Gayathri Nallathambi ◽  
V Sekar ◽  
Surendra kumar.M
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Potassium Hydrogen ◽  
Method Development And Validation ◽  
Development And Validation ◽  
High Degree

The aim of the study is to develop some new analytical method development and Validation of Quantitative Estimation of Anti-depressant Drug Vilazodone by UV and HPLC was found to be simple, specific, precise, accurate, rapid and economical. The method was developed and validated as per ICH guidelines, concerning accuracy, precision, linearity, ruggedness, limit of detection, limit of quantification and robustness and forced degradation studies. The GRACE ODS phenyl column (4.6 x 150mm,5μm) column was maintained at an ambient temperature and 232 nm λ max conditions. The mixture of di-potassium hydrogen phosphate with buffer (pH 7.4) and methanol in proportion 60:40v/v mobile phase was used in the flow rate of 1 ml/min. All validation methods shows good reproducibility and good recovery. The mean recoveries was found in the range between 99.6-99.9%. with % RSD values were within 2. The limit of detection and limit of quantification were found to be 0.05 μg/ml and 0.01 μg/ml respectively. The method was found to be having suitable application in routine laboratory analysis with high degree of accuracy and precision.

Chromatographic Quantification of Ivermectin and Pranziquantel in the Tablets Using Stability Indicating RP-HPLC Method

2019 ◽  
Vol 25 (3) ◽  
pp. 254-261
Author(s):  
Naga Venkata Suresh Kumar Devaka ◽  
Vallabhaneni Madhusudhan Rao
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard

Background: A new stability indicating RP-HPLC based assay method was developed to quantify ivermectin and praziquantel simultaneously and applied effectively to tablets. Methods: The simultaneous assay of ivermectin and praziquantel by RP-HPLC was done using an YMC C18 (250 mm × 4.6 mm, 5 µm) column with a mobile phase mixture of 0.1M disodium hydrogen phosphate (pH 4.5) and acetonitrile (55:45, v/v) using a isocratic flow rate of 1.0 ml/min and measured at 242 nm using photodiode array detector. All parameters were validated following the ICH guiding principles. The method was applied to quantify ivermectin and praziquantel simultaneously in tablets. Results: The retention values of ivermectin and praziquantel were 3.465 min and 4.468 min, respectively. The method’s linearity was found to be 1-3 µg/ml (ivermectin) and 25-75 µg/ml (praziquantel). The limit of detection was 0.010 µg/ml (ivermectin) and 0.046 µg/ml (praziquantel); limit of quantification was 0.033 µg/ml (ivermectin) and 0.155 µg/ml (praziquantel). The percent relative standard deviation of ivermectin and praziquantel was ˂1.0%. The percent assay was 99.51% and 99.20% for ivermectin and praziquantel, respectively. In tablets, the percent recovery of ivermectin and praziquantel was 99.60% and 99.38% with a percent relative standard deviation value of 0.353% and 0.106%, respectively. Stability indicating capability of the method was demonstrated through the stress degradation studies. Conclusion: The developed method was proved to be selective, precise and accurate for the quality control of ivermectin and praziquantel in tablets.

scholarly journals Development and Validation of UV Spectrophotometric Method of Mesalamine Using Hydrotropic Solubilizing Agents

2021 ◽  
Vol 12 (3) ◽  
pp. 2291-2296
Author(s):  
Bhavani N. L. D. ◽  
Gowtham Reddy Cheruku ◽  
Bhargava Sri Harsha Polina ◽  
Dheeraj Kotagiri ◽  
Jnanendra Kumar Korukollu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation

The work was proposed to discuss method development and validation of the drug Mesalamine by using hydrotropic solubilizing agents. An uncomplicated, accurate, and precise method was developed for the drug Mesalamine in bulk as well as Pharmaceutical dosage form. 5M Urea was used as the hydrotropic solubilizing agent to enhance the solubility of the drug. The maximum wavelength (ʎ max) for Mesalamine was found to be 241nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy, linearity, precision, Limit of detection (LOD) and Limit of quantification (LOQ). Percentage recovery (%) of Mesalamine was ascertained to be between 95 to 98%. Linearity for Mesalamine was observed between 2-10 µg/ml. Regression equation y=0.0571x-0.0186, regression coefficient (r²) is 0.9996 for Mesalamine. Inter day and intraday precision were checked, % relative standard deviation values were less than 2 for both the methods. Limit of detection (LOD) and Limit of quantification (LOQ) values were derived using regression equations. LOD value was found to be 0.55 µg/ml. LOQ value was found to be 1.67 µg/ml. The assay of the marketed formulation was performed and the results of the assay were obtained by the proposed method. The results are in between 98-102%. So, the method developed was simple and economical that can be adopted for routine tests.

APPLICATION OF EMISSION INTENSITY IN QUANTIFICATION AND FORCED DEGRADATION STUDIES OF MESALAMINE

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (03) ◽  
pp. 59-61
Author(s):  
Sunitha Gurrala ◽  
Panikumar D. Anumolu ◽  
Vasavi Panchakatla ◽  
Radhagayathri Achanta ◽  
Rajesh Chakka ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Alkaline Media ◽  
Forced Degradation ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Water As Solvent ◽  
Relative Standard ◽  
Forced Degradation Studies

A simple and sensitive spectrofluorimetric method has been developed for the estimation of mesalamine (MES). Linearity was obeyed in the range of 0.1-2.5 µg/mL in distilled water as solvent at an emission wavelength (λem) of 501 nm after excitation (λex) at 332 nm, with a good correlation coefficient of 0.999. The limit of detection and limit of quantification for this method were 0.05 and 0.1 µg/mL, respectively. The developed method was statistically validated as per ICH guidelines. The percentage relative standard deviation values were found to be less than 2 for accuracy and precision studies. The assay results obtained were in good agreement with the labeled amounts of the marketed formulations. This validated method was extended to study the degradation behavior of mesalamine in various conditions such as acid, alkaline, oxidative, thermal, and UV effects. Although there was no degradation observed in oxidative, thermal, UV effect, 41.9 % and 11.6 % amount was degraded in acid and alkaline media, respectively. The proposed method was effectively applied to routine quality control analysis of mesalamine in bulk and marketed formulations.

scholarly journals Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

2020 ◽  
Vol 18 (1) ◽  
pp. 962-973
Author(s):  
Saira Arif ◽  
Sadia Ata
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Fluocinolone Acetonide ◽  
Internal Diameter ◽  
Forced Degradation ◽  
Specific Method ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Relative Standard

AbstractA rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

Method Development and Validation of Spectrophotometric Methods for The Estimation of Rizatriptan Benzoate in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 6003-6006
Author(s):  
Pushpa Latha E. ◽  
Sailaja B.
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Analytical UV derivative spectrophotometric method was developed and validated to quantify Rizatriptan Benzoate in pure drug and tablet dosage form. Based on the spectrophotometric characteristics of Rizatriptan Benzoate, a signal of zero (225nm), first (216nm), second (237nm), third (233nm), fourth (231nm) order derivative spectra were found to be adequate for quantification. The methods obeyed Beer's law in the concentration range of (0.1-360µg/ml) with square correlation coefficient (r2) of 0.999. The mean percentage recovery was found to be 100.01 ± 0.075. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory.

scholarly journals Application of RP-HPLC for the Estimation of Allopurinol and Its Related Substances in Bulk and Tablet Dosage Form

2021 ◽  
pp. 11-20
Author(s):  
Ch. Jaswanth Kumar ◽  
Prachet Pinnamaneni ◽  
Siva Prasad Morla ◽  
K. N. Rajini Kanth ◽  
Rama Rao Nadendla
Keyword(s):  
Drug Testing ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Related Substances ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Aims: The main aim of the present study was to develop and validate a simple and cost- effective method for the estimation of allopurinol and its related substances by using RP-HPLC. Study Design:  Estimation of Allopurinol and its related substance in bulk and tablet dosage forms by RP-HPLC. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute of Pharmaceutical Sciences, Chalapathi Nagar, Lam, Guntur-522034 between October 2020 to January 2021. Methodology: Method development was carried out by using Schimadzu, Prominence-i series LC 3D-Plus autosampler embedded with lab solutions software, equipped with PDA detector using YMC column (150 mm X 4.6 mm, 3 μm) and 0.1M Ammonium acetate buffer as a mobile phase in the ratio of 100% at a flow rate of 1.0 ml/min at a wavelength of 255nm. The developed method was validated according to ICH guidelines. Results:  The linearity was observed in the range of 20-100 µg/ml with a regression (R2) value of 0.999. Developed method was specific with no interactions and accurate with 100.11% for allopurinol and 99.54% for its related substance. The limit of detection for allopurinol was 2 µg/ml and for related substance was 0.0.1 µg/ml. The limit of quantification for allopurinol was 6 µg/ml and for related substance was 0.03 µg/ml respectively. The percentage relative standard deviation was found to be NMT 2 which indicates that the proposed method was precise and robust. Conclusion:  The developed method was simple, precise and accurate and can be successfully employed for the estimation of allopurinol in bulk and tablet dosage form.

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.

Sign in / Sign up

Export Citation Format

Share Document