Analytical Method Development and Validation of Glipizide to Determine Residual solvents by head Space-Gas Chromatography

2021 ◽  
pp. 2440-2444
Author(s):  
Sanapala Srinivasa Rao ◽  
A. Vijayalakshmi
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Analytical Methodology ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Residual solvents in Pharmaceuticals are termed as organic volatile impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical methodology was developed for the quantification of residual solvents in Glipizide using a headspace gas chromatography (HSGC) with the help of flame ionization detector (FID). Methanol, acetone and dimethyl formamide as residual solvents were determined in Glipizide. Analysis was performed by headspace GC/FID method on Auto system- HS40. Nitrogen was used as a carrier gas and the separation of residual solvents was achieved by DB-Wax 0.25mm, 0.3mcm column. The thermostat temperature was 115 °C for 40 minutes for each vial. % RSD for nine injections obtained are in acceptance criteria. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated includes specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. According to the International Conference on Harmonization (ICH) guidelines, a new simple, specific, accurate and precise method was developed and validated.

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

scholarly journals Analytical method development and validation for simultaneous estimation of monoammonium glycyrrhizinate and sennoside-B in polyherbal laxative tablet using RP-HPLC

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Madhavi Patel ◽  
Shivangi Chauhan ◽  
Vishal Patel ◽  
Hardik Soni ◽  
Vikram Trivedi
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Determination Of Parameters ◽  
Development And Validation

Abstract Background Standardization of polyherbal medicine though being the need of the hour is a toilsome task. Among the various methods employed for quality control and standardization of polyherbal medicine, phytochemical profiling is of utmost importance as it signifies the quality as well as efficacy of the medicine. The work was aimed to develop and validate a simple, quick, and accurate RP-HPLC technique for simultaneous assessment of monoammonium glycyrrhizinate and sennoside-B in a polyherbal laxative tablet. The phytomarkers were effectively quantified by RP-HPLC system on C18 analytical column using gradient mobile phase consisting of phosphate buffer to acetonitrile with the detector wavelength set at 254 nm. This developed method was validated by determination of parameters like accuracy, linearity, precision, limit of detection, and quantification as well as robustness according to ICH guidelines. Results Calibration curve of both phytomarkers showed excellent linear correlation coefficients. LOD and LOQ were also calculated by equation. Precision studies were carried out using intra-day and inter-day intervals and RSD values were found to be less than 2.00%. The method was found to be accurate, which was evident from 98.96 to 101.39% and 99.17 to 100.67% recovery of monoammonium glycyrrhizinate and sennoside-B, respectively, when the formulation was spiked with the respective phytomarkers. Conclusion The validated method can be employed as standardization tool for herbal formulations with accuracy and precision. The developed method will assist in maintaining the good quality and batch to batch uniformity of polyherbal formulations containing Yashtimadhu, Swarnpatri, and Aragvadha as active ingredients.

scholarly journals Development and Validation of a Headspace Gas Chromatographic (HS-GC) Method for Determination of Residual Solvents in Nitazoxanide API

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 1719-1727
Author(s):  
Rajesh Kumar Chawla ◽  
Koteswara Rao G S N ◽  
Umasankar Kulandaivelu ◽  
Siva Prasad Panda ◽  
Rajasekhar Reddy Alavala
Keyword(s):  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Limit Of Quantification ◽  
Residual Solvents ◽  
Pharmaceutical Ingredients ◽  
Quality Control Laboratory ◽  
Ich Guidelines ◽  
Headspace Gas ◽  
Development And Validation

Controlling residual solvents in the drug substances or active pharmaceutical ingredients (API) is mandatory to the specified limits as per the International Conference on Harmonisation (ICH) Q3C guidelines. Residual solvents in pharmaceuticals are mostly determined by Gas Chromatography with Headspace. A simple and sensitive headspace gas chromatographic (HS-GC) method has been developed for the determination of Acetone, Dichloromethane and Cyclohexane in Nitazoxanide API. The separation of analytes was achieved with DB – 624 (30 m length, 0.53 mm inner diameter and 3.0 μm in film thickness) capillary column. Dimethyl formamide was used as a diluent. Nitrogen was used as carrier gas with 3.0 mL/minutes and Flame ionisation detector (FID) for detecting analytes. The oven temperature was set at 60°C for 5 minutes at initial and programmed at a rate of 20°C per minute to a final temperature of 240°C for 2 minutes. Run time was 16 minutes, and total GC cycle time was 25 minutes. The spilt ratio used as 1:20 to get optimum peak response. The developed method was validated as per the ICH guidelines for specificity, accuracy, precision, linearity, range, the limit of detection, the limit of quantification and robustness. The results of validation were indicated no interference, good recoveries, precise, linear, rugged and robust method, suitable for the determination of residual solvents in Nitazoxanide API for research and routine quality control laboratory.

scholarly journals UV Method Development and Validation of Ellagic Acid for its Rapid Quantitative Estimation

2019 ◽  
Vol 7 (1) ◽  
pp. 1-5
Author(s):  
Harsheen Kaur ◽  
Arti Thakkar ◽  
Kalpana Nagpal
Keyword(s):  
Ellagic Acid ◽  
Method Development ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Uv Spectroscopy ◽  
Entrapment Efficiency ◽  
Good Recovery ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Development and validation of a simple UV- Spectroscopy method was done for the quantitative analysis of Ellagic Acid (EA). The stock solution of 50μg/ml was prepared and scanned, for which absorption maxima was found to be 277nm. Further dilutions to different concentrations (1-5μg/ml) were prepared and analyzed at 277nm. The method so developed was validated as per ICH guidelines for: linearity, robustness, precision, accuracy, limit of detection and quantification. The Lambert- Beer’s law is followed in the range (1-5μg/ml) with correlation coefficient value 0.9994. It was observed that the method is precise and accurate for EA analysis with good recovery percent of 94.47% to 106.83%. The method developed was further employed for determining the entrapment efficiency of ellagic acid and its release from its nanoparticle dosage form. The method may be utilized for determining the concentration of EA when present as formulation and in combination with other drugs.

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.

RAPID RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF LURASIDONE HYHROCHLORIDE IN BULK AND TABLET FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 28-34
Author(s):  
K. Vijaya Sri ◽  
M. Shiva Kumar ◽  
A. Sravani ◽  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Tablet Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

The RP-HPLC were developed and validated for the estimation of lurasidone HCl as per ICH guidelines. A simple, fast, accurate and precise RP-HPLC method was developed by using methanol: water containing 0.01% ortho phosphoric acid in the ratio of 70:30 (V/V). The method was developed in Eclipse C18 column (100 mm × 4.6 mm, 3.5 μm particle size). The method was found to be linear in the range of 2.5- 15µg/mL with a correlation coefficient value of 0.999. The accuracy studies of RP-HPLC method was performed at three different levels, i.e., 50%, 100%, and 150% and recovery was found to be in the range of 100.1-100.6% .The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.30-0.92. Satisfactory validation was also obtained from recovery (99.8%) studies, intra-day and interday precision and robustness 2%. The proposed method was found to be accurate, precise and rapid for the analysis of lurasidone.

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.

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.

Sign in / Sign up

Export Citation Format

Share Document