Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry
| Autor: | Yasuhiro Fujiwara, Kazuichi Umemoto, Koji Urakami, Yuka Saito, Chuichi Watanabe, Masayuki Godo, Keiji Hashimoto |
|---|---|
| Rok vydání: | 2001 |
| Předmět: |
Quality Control
Chromatography Chemistry Chemistry Pharmaceutical Thermal desorption Analytical chemistry Temperature General Chemistry General Medicine Reference Standards Mass spectrometry Gas Chromatography-Mass Spectrometry Solvent Pharmaceutical Preparations Desorption Drug Discovery Melting point Solvents Gas chromatography Gas chromatography–mass spectrometry Drug Contamination Quantitative analysis (chemistry) |
| Zdroj: | Chemicalpharmaceutical bulletin. 48(12) |
| ISSN: | 0009-2363 |
| Popis: | Thermal desorption (TD) techniques followed by capillary GC/MS were applied for the analysis of residual solvents in bulk pharmaceuticals. Solvents desorbed from samples by heating were cryofocused at the head of a capillary column prior to GC/MS analysis. This method requires a very small amount of sample and no sample pretreatment. Desorption temperature was set at the point about 20 degrees C higher than the melting point of each sample individually. The relative standard deviations of this method tested by performing six consecutive analyses of 8 different samples were 1.1 to 3.1%, and analytical results of residual solvents were in agreement with those obtained by direct injection of N,N-dimethylformamide solution of the samples into the GC. This novel TD/GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents in bulk pharmaceuticals. |
| Databáze: | OpenAIRE |
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