Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry.
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.
Urakami
K
K
Analysis & Quality Control Department, Takeda Chemical Industries, Ltd, Osaka, Japan. Urakami_Koji@takeda.co.jp
Saito
Y
Y
Fujiwara
Y
Y
Watanabe
C
C
Umemoto
K
K
Godo
M
M
Hashimoto
K
K
D002626:Chemistry, Pharmaceutical / Q000379:methods; D004340:Drug Contamination; D008401:Gas Chromatography-Mass Spectrometry; D004364:Pharmaceutical Preparations / Q000032:analysis*; D011786:Quality Control; D012015:Reference Standards; D012997:Solvents / Q000032:analysis*; D013696:Temperature
D004364:Pharmaceutical Preparations; D012997:Solvents