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

Pharmacia ◽  
2021 ◽  
Vol 68 (1) ◽  
pp. 53-59
Author(s):  
Оlena Golembiovska ◽  
Oleksii Voskoboinik ◽  
Galina Berest ◽  
Sergiy Kovalenko ◽  
Liliya Logoyda
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Accurate Method ◽  
Chromatography Method ◽  
Synthetic Process ◽  
Residual Solvent ◽  
Residual Solvents ◽  
All Solutions ◽  
Limit Of Quantitation

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.

Fast Method for the Determination of Residual Solvents in Radiopharmaceutical Products

2017 ◽  
Vol 68 (4) ◽  
pp. 666-670 ◽  
Author(s):  
Mirela Mihon ◽  
Catalin Stelian Tuta ◽  
Alina Catrinel Ion ◽  
Dana Niculae ◽  
Vasile Lavric
Keyword(s):  
Gas Chromatography ◽  
Control Method ◽  
Limit Of Detection ◽  
The Body ◽  
Biologically Active ◽  
Injection Technique ◽  
Fast Method ◽  
Residual Solvent ◽  
Residual Solvents

The aim of this work was the development and validation of a fast analytical method to determine the residual solvents content in radiopharmaceuticals such as: 18F-Fluorodeoxyglucose (18F-FDG), 18F-Fluoroestradiol (18F-FES), 18F-Fluorothymidine (18F-FLT),18F-Fluoromisonidazole (18F-FMISO). Radiopharmaceuticals are radioactive preparations for medical purposes used in nuclear medicine as tracers in diagnostic imaging and treatment of certain diseases. Positron Emission Tomography (PET) is a medical imaging technique that consists in introducing into the body of a small amount of a biologically active chemical compound labelled with a short lived positron-emitting radioisotope (18F, 11C, 68Ga). Residual solvents are critical impurities in radiopharmaceuticals that can affect labelling, stability and physicochemical properties of drugs. Therefore, the determination of these solvents is essential for quality control of radiopharmaceuticals. Validation of the control method for residual solvents by gas chromatography is referred by the European Pharmacopoeia using a special injection technique (head space). The parameters of the method, which comply with International Conference on Harmonization guidelines, are: accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The proposed method (direct gas chromatography injection) proved to be linear, precise, accurate and robust. Good linearity was achieved for all the solvents and correlation coefficients (R2) for each residual solvent were found more than 0.99.

Method of Validation for Residual Solvents in Bisoprolol Fumarate by GC Technique

2021 ◽  
pp. 147-155
Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Technique ◽  
Range Limit ◽  
Column Temperature ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Chromatographic Condition ◽  
Methylene Dichloride

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.

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.

Development and Validation of Head-space Gas Chromatographic Method in Tandem with Flame ionized detection for the determination of Residual solvents in Simeprevir API Synthesis

2021 ◽  
pp. 5175-5181
Author(s):  
C. Hazarathaiah Yadav ◽  
A. Malli Babu
Keyword(s):  
Limit Of Detection ◽  
Intermediate Precision ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Limit Of Quantitation ◽  
Reference Material Certification ◽  
Precision System ◽  
Gas Chromatographic Method ◽  
Development And Validation

Residual solvent testing is an integral part of reference material certification. A gas chromatography/flame ionization detector/headspace method has been developed and validated to detect and quantitate commonly used residual solvents in our production processes: Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir API. A simple and selective HS-GC method is described for the determination & quantification of Residual Solvents in Simeprevir API. Chromatographic separation was achieved on USP G43 equivalent capillary column Thermo Scientific™ Trace GOLD™ TG-624 SilMS, 30m × 0.32mm × 1.8µm column (P/N 26059-3390) using nitrogen as carrier gas by using different temperature gradient of FID Detectors. Linearity was observed in the range 40-120% of standard concentrations for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane (r2>0.999) for the amount of solvent estimated by the proposed methods was in good agreement. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered diluent and API. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 10 for Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical active ingredients for estimation of Residual Solvents of Methanol, Tetrahydrofuran, Toluene, Dichloromethane and Dichloroethane in Simeprevir. Baseline separation of all five solvents and Simeprevir API is achieved within 20.5 minutes of analysis time. Method validation comprised the following parameters: limit of detection (LOD), limit of quantitation (LOQ), linearity and range, accuracy, precision (repeatability and intermediate precision), system suitability, specificity, and robustness. Linearity and LOQ (ppm) are listed for each solvent in manuscript. The present method was proven to be robust and accurate for quantitative analysis of residual solvent in neat materials.

Development and Validation of an Automated Gas Chromatography Method for Determination of Dichloromethane in Ampicillin Sodium by Using Capillary Column Technology

2020 ◽  
Vol 16 (7) ◽  
pp. 901-908
Author(s):  
Manisha Trivedi ◽  
Elsy Raynil John ◽  
Faraat Ali ◽  
Anuj Prakash ◽  
Robin Kumar ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Direct Injection ◽  
High Sensitivity ◽  
Chromatography Method ◽  
Ampicillin Sodium ◽  
Static Headspace Gas Chromatography ◽  
Limit Of Quantitation

Background: The main aim of the study was to develop an automated static headspace gas chromatography (SHS-GC) method for determination of dichloromethane (DCM) in ampicillin sodium by using a capillary column. Methods: SHS-GC also known as gas chromatography-headspace is the technique of choice due to its high sensitivity, excellent separation abilities, low limit of detection and simplicity of the instrumentation used for the technique. The headspace sampling method has more appropriate sensitivity than the direct injection method because it can clearly separate volatile analytes from the sample matrix and effectively concentrate them. Therefore, this method results in less complex sample preparation, decreased instrument contamination, and increased capillary column life. Results: The developed SHS-GC method showed symmetrical peak shape reasonable retention time for DCM. A linear relationship was obtained over the range of 2-240 μg mL-1 with a correlation coefficient (r2) of 0.993. The recovery, system precision and robustness of the method were within the acceptable values. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were 0.5 μg mL-1 and 2 μg mL-1 respectively. Conclusions: The results obtained in this study demonstrate that SHS-GC method is selective, precise, linear, accurate and robust for determination of dichloromethane in ampicillin sodium and its formulation (injection).

scholarly journals ANALYSIS OF DETERMINING CONCENTRATION OF 3QUINUCLIDINOL IN DRUG SUBSTANCES

2020 ◽  
Vol 2 (2) ◽  
pp. 60-65
Author(s):  
Abdul Qadeer ◽  
Yaseen Jan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Sodium Hydroxide Solution ◽  
Drug Substance ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Drug Substances ◽  
Solifenacin Succinate ◽  
Validation Criteria

The goal of the study was to determine low level concentrations of 3-quinuclidinol in solifenacin succinate drug substance by using gas chromatography system. 3-quinuclidinol was used as an intermediate in the process of synthesis of solifenacin succinate. The method development was initiated with solifenacin succinate, solubility of 3-quinuclidinol, extraction and miscibility studies, chosen with 6 N sodium hydroxide solution and chloroform solvents. The method of the study was validated based on the guidelines provided by ICH. The criteria were method precision, robustness, accuracy, linearity, limit of quantification, limit of detection, and individuality in terms of specificity. In conclusion, in the present study, we developed a reliable gas chromatography method which was validated based on 3quinuclidinol in solifenacin succinate drug substance. Findings of different validation criteria used shows that the proposed method in this study is accurate, robust, precise, linear, sensitive, and specific.

FORCED INDICATING UPLC-DAD METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF APALUTAMIDE IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (09) ◽  
pp. 73-75
Author(s):  
China Babu D ◽  
Madhusudhana Chetty C ◽  
Mastanamma S. K ◽  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Uv Light ◽  
Accurate Method ◽  
Pharmaceutical Dosage Form ◽  
Good Ability ◽  
Acquity Uplc ◽  
Development And Validation

A new analytical method was developed for the estimation of apalutamide in bulk and its pharmaceutical formulation. The sensitive, précise and accurate method was developed by using Waters Acquity UPLC system equipped with quaternary gradient pump. The column used was Waters C18 150 X 2.1 mm X 1.7 µm and mobile phase was 0.2 % OPA buffer in water : acetonitrile in the ratio of 25:75 V/V. The buffer pH was maintained at 4.5. The fl ow rate of mobile phase was 0.5 mL min-1 and detection was at 272 nm by using PDA detector. The method was performed at ambient temperature. The retention time of the apalutamide was 1.27 min. The % RSD value in precision was >2 %. The accuracy of the method was found to be between 99.54 % - 100.01 %. The limit of detection and limit of quantifi cation values were found to be 0.14 µg mL-1 and 0.48 µg mL-1, respectively. The linearity concentration range was found to be 11.25 - 67.5 µg mL-1, it show wide linearity concentration range. The method was proved to have good robustness after changing parameters of fl ow rate, temperature and mobile phase composition. The method showed good ability towards different stress conditions of acidity, alkalinity, peroxide and UV-light. The method can be used for the routine analysis of apalutamide in bulk and its pharmaceutical dosage form by using UPLC.

Brazilian southeast brown propolis: gas chromatography method development for its volatile oil analysis, its antimicrobial and leishmanicidal activities evaluation

2020 ◽  
Vol 32 (3) ◽  
pp. 404-411
Author(s):  
Victor Pena Ribeiro ◽  
Caroline Arruda ◽  
Jennyfer Andrea Aldana Mejía ◽  
Ana Carolina Bolela Bovo Candido ◽  
Raquel Alves Santos ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Volatile Oil ◽  
Oil Analysis ◽  
Chromatography Method

scholarly journals Residual solvent determination by head space gas chromatography with flame ionization detector in omeprazole API

2011 ◽  
Vol 47 (2) ◽  
pp. 379-384 ◽  
Author(s):  
Saurabh Pandey ◽  
Preeti Pandey ◽  
Raj Kumar ◽  
Narendra Pal Singh
Keyword(s):  
Gas Chromatography ◽  
Active Pharmaceutical Ingredient ◽  
Reversible Inhibitor ◽  
Internal Diameter ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Pharmaceutical Ingredients ◽  
Flame Ionization ◽  
Head Space ◽  
Head Space Gas Chromatography

Residual solvents in pharmaceutical samples are monitored using gas chromatography with head space. Based on good manufacturing practices, measuring residual solvents is mandatory for the release testing of all active pharmaceutical ingredients (API). The analysis of residual organic solvents (methanol, acetone, cyclohexane, dichloromethane, toluene) in Omeprazole, an active pharmaceutical ingredient was investigated. Omeprazole is a potent reversible inhibitor of the gastric proton pump H+/K+-ATPase. The Head space gas chromatography (HSGC) method described in this investigation utilized a SPB TM-624, Supelco, 30 m long x 0.25 mm internal diameter, 1.4µm-thick column. Since Omeprazole is a thermally labile compound, the selection of the proper injector temperature is critical to the success of the analysis. The injector temperature was set at 170ºC to prevent degradation. The initial oven temperature was set at 40ºC for 12 min and programmed at a rate of 10ºC min-1 to a final temperature of 220ºC for 5 min. Nitrogen was used as a carrier gas. The sample solvent selected was N,N-dimethylacetamide. The method was validated to be specific, linear, precise, sensitive, rugged and showed excellent recovery.

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