{"title":"Dynamic extraction of residual solvents from pharmaceutical formulations using a needle-type extraction device.","authors":"Ikuo Ueta, Daisuke Kondo, Suguru Masuda, Yuki Ariizumi, Ryosuke Kikuchi, Koki Nakagami, Yoshihiro Saito","doi":"10.1007/s44211-024-00674-9","DOIUrl":null,"url":null,"abstract":"<p><p>This study developed a rapid screening method to determine residual solvents contained in a tablet formulation using a needle-type extraction device. For this, the tablet formulation was pulverized and the powdered sample was rapidly inserted into a pipette tip. After fixing the sample with quartz wool, the pipette tip was capped with a silicon septum. A needle-type extraction device packed with Carbopack X and a carbon molecular sieve was inserted into the pipette tip through the septum, and the gas sample was collected. During this gas sampling, pure N<sub>2</sub> gas was introduced into the pipette tip. The extraction time for collecting 100 mL of the sample was approximately 10 min. After gas sampling, the extraction needle was connected to a gas-tight syringe and 0.5 mL of pure N<sub>2</sub> gas (desorption gas) was collected. The extraction needle was then inserted into a heated gas chromatographic injection port. The extracted residual solvents were then thermally desorbed and determined using a gas chromatograph-flame ionization detector. The detector response is very low for carbon tetrachloride, although the proposed method showed sufficient sensitivity for five Class 1 compounds. Additionally, this study clearly indicated that the purge efficiency of residual solves with dynamic extraction is different between powdered pharmaceutical formulations.</p>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":null,"pages":null},"PeriodicalIF":1.8000,"publicationDate":"2024-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analytical Sciences","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1007/s44211-024-00674-9","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
Abstract
This study developed a rapid screening method to determine residual solvents contained in a tablet formulation using a needle-type extraction device. For this, the tablet formulation was pulverized and the powdered sample was rapidly inserted into a pipette tip. After fixing the sample with quartz wool, the pipette tip was capped with a silicon septum. A needle-type extraction device packed with Carbopack X and a carbon molecular sieve was inserted into the pipette tip through the septum, and the gas sample was collected. During this gas sampling, pure N2 gas was introduced into the pipette tip. The extraction time for collecting 100 mL of the sample was approximately 10 min. After gas sampling, the extraction needle was connected to a gas-tight syringe and 0.5 mL of pure N2 gas (desorption gas) was collected. The extraction needle was then inserted into a heated gas chromatographic injection port. The extracted residual solvents were then thermally desorbed and determined using a gas chromatograph-flame ionization detector. The detector response is very low for carbon tetrachloride, although the proposed method showed sufficient sensitivity for five Class 1 compounds. Additionally, this study clearly indicated that the purge efficiency of residual solves with dynamic extraction is different between powdered pharmaceutical formulations.
期刊介绍:
Analytical Sciences is an international journal published monthly by The Japan Society for Analytical Chemistry. The journal publishes papers on all aspects of the theory and practice of analytical sciences, including fundamental and applied, inorganic and organic, wet chemical and instrumental methods.
This publication is supported in part by the Grant-in-Aid for Publication of Scientific Research Result of the Japanese Ministry of Education, Culture, Sports, Science and Technology.