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  • 标题:High Sensitivity Analysis of Indirubin by Silylation Using GC/MS
  • 作者:Yuji Takao ; Kohei Yamashita ; Shinya Kohra
  • 期刊名称:Journal of Health Science
  • 印刷版ISSN:1344-9702
  • 电子版ISSN:1347-5207
  • 出版年度:2003
  • 卷号:49
  • 期号:1
  • 页码:88-90
  • DOI:10.1248/jhs.49.88
  • 出版社:The Pharmaceutical Society of Japan
  • 摘要:After adding the silylating agents N, O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) or N-methyl-N-(tert-butyldimethylsilyl) trifluoroacetamide (MTBSTFA) to the indirubin solution and leaving for 1 hr at 60°C, the color remained red. Indirubin could be measured by GC/MS after replacing the active hydrogen on the amino group with -Si(CH3)3 or -Si(CH3)2C2H5 groups. However, peak tailing was observed and the quantitative and detection limits were not sensitive enough for practical use. Indirubin silylated at four sites was observed under the reaction conditions as follows; solvent dichloromethane: acetone (8 : 2), 90°C reaction temperature, 1 hr reaction time, BSTFA derivative, pyridine catalyst. The color of the solution changed from red to colorless. Retention time appeared to be faster and the peak shape improved. Under these conditions, the quantitative and detection limits of indirubin were 5 ppb and 0.1 ppb, respectively.
  • 关键词:indirubin;silylation;GC/MS;N, O-bis(trimethylsilyl) trifluoroacetamide;derivative
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