Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2

Aim. The aim of study was to develop and validate a simple, precise and accurate method using gas chromatography for analysis of residual solvents – acetone and 2-propanol – in quinabut API. Materials and methods. All experiments were performed on a gas chr...

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Main Authors: Оlena Golembiovska, Oleksii Voskoboinik, Galina Berest, Sergiy Kovalenko, Liliya Logoyda
Format: Article
Language:English
Published: Pensoft Publishers 2021-01-01
Series:Pharmacia
Online Access:https://pharmacia.pensoft.net/article/52119/download/pdf/
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spelling doaj-c728ca4e03f34019ac1b50d281db87c72021-09-28T14:38:55ZengPensoft PublishersPharmacia2603-557X2021-01-01681535910.3897/pharmacia.68.e5211952119Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2Оlena Golembiovska0Oleksii Voskoboinik1Galina Berest2Sergiy Kovalenko3Liliya Logoyda4National Technical University of Ukraine "Igor Sikorsky Kyiv Polytechnic Institute"Zaporizhzhya State Medical UniversityZaporizhzhya State Medical UniversityZaporizhzhya State Medical UniversityI. Horbachevsky Ternopil State Medical University Aim. The aim of study was to develop and validate a simple, precise and accurate method using gas chromatography for analysis of residual solvents – acetone and 2-propanol – in quinabut API. Materials and methods. All experiments were performed on a gas chromatographic system equipped with FID detector (Shimadzu GC System) using the DB-624 (30 m × 0.32 mm ID, 3.0 μm film sickness) column as stationary phase. Nitrogen was used as carrier gas with flow rate 7.5 mL/ min. Split ratio was 1:5, injector temperature was 140 °C, detector temperature was 250 °C, oven temperature was programmed from 40 °C (2 min) to 50 °C at 1 °C/min and then increased at a rate of 15 °C/min up to 215 °C; and maintained for 2 min. All solutions were prepared using water as diluent. Results. This proposed method is assessed for separation of residual solvent from quinabut with quantification. The obtained results are compared with the corresponding specified limits of ICH standard guidelines. The method validation was done by evaluating specificity, limit of detection (LOD) and limit of quantitation (LOQ), linearity, accuracy, repeatability, ruggedness, system suitability and method precision of residual solvents as indicated in the ICH harmonized tripartite guideline. The separation between acetone and 2-propanol peaks is 2.07. Hence method was found to be specific. The linear relationship evaluated across range of 15 to 180% for acetone and 2-propanol of ICH specified limit of residual solvents. The graphs of theoretical concentration versus obtained concentration are linear and the regression coefficients ‘R’ for residual solvents were more than 0.9968. The values of LOD and LOQ were much less than the lower limit of the concentration range and cannot affect the accuracy of the test. The technique was characterized by high intra-laboratory accuracy at concentrations close to the nominal acetone and 2-propanol concentration. All solutions were stable in water for at least 1 hour when stored at room temperature. Conclusion. A simple, specific, accurate, precise and rugged gas chromatography method was developed and validated for the quantification of residual solvents present in quinabut API through an understanding of the synthetic process, nature of solvents and nature of stationary phases of columns. The residual solvents acetone and 2-propanol were determined. https://pharmacia.pensoft.net/article/52119/download/pdf/
collection DOAJ
language English
format Article
sources DOAJ
author Оlena Golembiovska
Oleksii Voskoboinik
Galina Berest
Sergiy Kovalenko
Liliya Logoyda
spellingShingle Оlena Golembiovska
Oleksii Voskoboinik
Galina Berest
Sergiy Kovalenko
Liliya Logoyda
Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
Pharmacia
author_facet Оlena Golembiovska
Oleksii Voskoboinik
Galina Berest
Sergiy Kovalenko
Liliya Logoyda
author_sort Оlena Golembiovska
title Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
title_short Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
title_full Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
title_fullStr Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
title_full_unstemmed Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2
title_sort method development and validation for the determination of residual solvents in quinabut api by using gas chromatography. message 2
publisher Pensoft Publishers
series Pharmacia
issn 2603-557X
publishDate 2021-01-01
description Aim. The aim of study was to develop and validate a simple, precise and accurate method using gas chromatography for analysis of residual solvents – acetone and 2-propanol – in quinabut API. Materials and methods. All experiments were performed on a gas chromatographic system equipped with FID detector (Shimadzu GC System) using the DB-624 (30 m × 0.32 mm ID, 3.0 μm film sickness) column as stationary phase. Nitrogen was used as carrier gas with flow rate 7.5 mL/ min. Split ratio was 1:5, injector temperature was 140 °C, detector temperature was 250 °C, oven temperature was programmed from 40 °C (2 min) to 50 °C at 1 °C/min and then increased at a rate of 15 °C/min up to 215 °C; and maintained for 2 min. All solutions were prepared using water as diluent. Results. This proposed method is assessed for separation of residual solvent from quinabut with quantification. The obtained results are compared with the corresponding specified limits of ICH standard guidelines. The method validation was done by evaluating specificity, limit of detection (LOD) and limit of quantitation (LOQ), linearity, accuracy, repeatability, ruggedness, system suitability and method precision of residual solvents as indicated in the ICH harmonized tripartite guideline. The separation between acetone and 2-propanol peaks is 2.07. Hence method was found to be specific. The linear relationship evaluated across range of 15 to 180% for acetone and 2-propanol of ICH specified limit of residual solvents. The graphs of theoretical concentration versus obtained concentration are linear and the regression coefficients ‘R’ for residual solvents were more than 0.9968. The values of LOD and LOQ were much less than the lower limit of the concentration range and cannot affect the accuracy of the test. The technique was characterized by high intra-laboratory accuracy at concentrations close to the nominal acetone and 2-propanol concentration. All solutions were stable in water for at least 1 hour when stored at room temperature. Conclusion. A simple, specific, accurate, precise and rugged gas chromatography method was developed and validated for the quantification of residual solvents present in quinabut API through an understanding of the synthetic process, nature of solvents and nature of stationary phases of columns. The residual solvents acetone and 2-propanol were determined.
url https://pharmacia.pensoft.net/article/52119/download/pdf/
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