Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry |
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Authors: | Urakami K Saito Y Fujiwara Y Watanabe C Umemoto K Godo M Hashimoto K |
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Affiliation: | Analysis & Quality Control Department, Takeda Chemical Industries, Ltd, Osaka, Japan. Urakami_Koji@takeda.co.jp |
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Abstract: | 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. |
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