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 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.

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.

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.

scholarly journals Development and Validation of a Simple Method for Routine Analysis of Ractopamine Hydrochloride in Raw Material and Feed Additives by HPLC

2009 ◽  
Vol 92 (3) ◽  
pp. 757-764 ◽  
Author(s):  
Ellen Figueiredo Freire ◽  
Keyller Bastos Borges ◽  
Hélio Tanimoto ◽  
Raquel Tassara Nogueira ◽  
Lucimara Cristiane Toso Bertolini ◽  
...  
Keyword(s):  
Quality Control ◽  
Limit Of Detection ◽  
Feed Additives ◽  
Raw Material ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Relative Standard ◽  
Validation Parameters ◽  
Ractopamine Hydrochloride

Abstract A simple method was optimized and validated for determination of ractopamine hydrochloride (RAC) in raw material and feed additives by HPLC for use in quality control in veterinary industries. The best-optimized conditions were a C8 column (250 4.6 mm id, 5.0 m particle size) at room temperature with acetonitrile100 mM sodium acetate buffer (pH 5.0; 75 + 25, v/v) mobile phase at a flow rate of 1.0 mL/min and UV detection at 275 nm. With these conditions, the retention time of RAC was around 5.2 min, and standard curves were linear in the concentration range of 160240 g/mL (correlation coefficient 0.999). Validation parameters, such as selectivity, linearity, limit of detection (ranged from 1.60 to 2.05 g/mL), limit of quantification (ranged from 4.26 to 6.84 g/mL), precision (relative standard deviation 1.87), accuracy (ranged from 96.97 to 100.54), and robustness, gave results within acceptable ranges. Therefore, the developed method can be successfully applied for the routine quality control analysis of raw material and feed additives.

scholarly journals ANALYTICAL METHOD DEVELOPMENT, VALIDATION AND FORCED DEGRADATION STUDIES OF LANSOPRAZOLE BY RP-HPLC

2018 ◽  
Vol 6 (4) ◽  
pp. 21-29
Author(s):  
Madhavi K Meher ◽  
Charushila Bhangale ◽  
Ramdas Dholas ◽  
Vandana Aher Prashant ◽  
Rohan Pawar
Keyword(s):  
Chromatographic Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Reciprocating Pump ◽  
Liquid Chromatographic

The objective of this work is to develop a rapid, precise, accurate and sensitive revere phase liquid chromatographic method and Forced degradation studies for the estimation of Lansoprazole. The chromatographic method was standardized for Lansoprazole using Shimadzu HPLC model reverse phase analytical Inspire grace C18 column (250 mm x 4.5 mm, 5mm particle size) with PC-3000-M Reciprocating Pump (40 Mpa) and UV-3000-M Detector, at 285nm and flow rate of 0.8 ml/min. The mobile phase consists of 80:20 Methanol: water. The linearity of proposed method was investigated in the range of 10-50 µm/ml (R2 = 0.999) of Lansoprazole. The limit of detection (LOD) was found to be 0.12 mm/ml. The limit of quantification (LOQ) was found to be 0.36 mg/ml. The retention time of Lansoprazole found to be 5.4 min. The method was statistically validated and % RSD was found to be less than 2 indicating high degree of accuracy and precision. Hence proposed method can be successfully applied for the estimation of Lansoprazole in further studies. Keywords: Lansoprazole, RP-HPLC, Chromatogram, validation, estimation.

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 Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals Spectrophotometric Method for the Determination of Drugs Containing Phenol Group by Using 2, 4- Dinitrophenylhydrazine

2010 ◽  
Vol 7 (2) ◽  
pp. 395-402
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Kumar Shrestha
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Phenolic Drugs

A spectrophotometric method has been proposed for the determination of four phenolic drugs; salbutamol, ritodrine, amoxicillin and isoxsuprine. The method is based on the oxidation of 2, 4- dinitrophenyl-hydrazine and coupling of the oxidized product with drugs to give intensely colored chromogen. Under the proposed optimum condition, beer’s law was obeyed in the concentration range of 2.5-17, 2-29, 4-33 and 5-30 μg/mL for salbutamol, ritodrine, amoxicillin and isoxsuprine respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 0.2, 0.83, 0.09, 0.84 μg/mL and 0.66, 2.79, 0.3 and 2.81 μg/mL in the same order. No interference was observed from common pharmaceutical adjuvants. The ringbom plots and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical dosage forms, which was compared statistically with reference methods by means oft- test andF- test and were found not to differ significantly at 95% confidence level. The procedure is characterized by its simplicity with accuracy and precision.

scholarly journals UV Spectrophotometric Methods to Quantify Alogliptin Benzoate and Pioglitazone Hydrochloride

2021 ◽  
pp. 31-41
Author(s):  
Dhanya B. Sen ◽  
Ashim K. Sen ◽  
Aarti S. Zanwar ◽  
Harshita Pandey ◽  
Rajesh A. Maheshwari
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ich Guidelines ◽  
The Difference ◽  
Tablet Dosage

Three new, precise, accurate and sensitive UV-Spectrophotometric methods namely Ratio Difference Spectroscopic Method (RDSM), First Derivative of Ratio Spectra Method (DR1) and Area Under Curve Method (AUC) were developed and validated for simultaneous assessment of alogliptin benzoate (ALO) and pioglitazone hydrochloride (PIO) in tablet dosage form. In RDSM, ratio spectra of both the drugs were recorded by dividing the mixtures using interfering drug as divisor. Then the difference between the amplitudes of obtained ratio spectra was measured at 288 and 291 nm for ALO and 236 and 245 nm for PIO. The second method DR1, where the first derivative of ratio spectra of both the drugs were recorded and the first derivative signal was measured at 290 nm for ALO and 276.8 nm for PIO. The scaling factor was fixed as 1 and wavelength interval (Δλ) as 2 for recording the first derivative of ratio spectra.  In the third method (AUC), peak area of recorded zero order spectra was measured at 276 ± 10 nm for ALO and 267.8 ± 10 nm for PIO. All three proposed methods were validated according to “International Conference on Harmonization” (ICH) guidelines parameters. For all three methods, ALO and PIO obeyed Beer’s law in the range of 0.5-5 & 1.8-18 µg/ml, respectively. The % RSD of repeatability of measurement, intra-day and inter-day precision were found to be less than 2 for all three methods. Limit of detection (LOD) and Limit of quantification (LOQ) of the drugs were calculated which proved the sensitivity of the methods. The accuracy ranged between 98-101% for all three methods. No interference from pharmaceutical excipients present in the formulation was observed.  These proposed methods were found to be simple, sensitive, accurate and precise and can be applied to the simultaneous estimation of ALO and PIO in combined tablet formulation and also appropriate for routine quality control analysis.

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.

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