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J.Health Sci., 49(1), 88-90, 2003
High Sensitivity Analysis of Indirubin by Silylation Using
GC/MS
Yuji Takao,*, a Kohei
Yamashita,a Shinya
Kohra,a Makiko
Inudo,b Masaki
Nagae,a
Nobuaki Tominaga,c Yasuhiro
Ishibashi,d Jun
Sekizawa,e Shinichi
Miyairi,f
and Koji Arizonob
aFaculty of Environmental Studies, Nagasaki University, Bunkyo-machi, 1-14, Nagasaki 852-8521, Japan, bFaculty of
Environmental and Symbiotic Sciences, Prefectural University of Kumamoto, 3-1-100 Tsukide, Kumamoto 862-8502 Japan,
cDepartment of Chemical and Biological Engineering, Ariake National College of Technology, 150 Higashihagino-machi,
Omuta 836-8585, Japan, dEnvironmental Protection Center, Nagasaki University, Bunkyo-machi, 1-14, Nagasaki 852-8521,
Japan, eDivision of Chem-Bio Informatics, National Institute of Health Sciences, Kamiyoga 1-18-1, Setagaya-ku, Tokyo
158-8501, Japan, and fCollege of Pharmacy, Nihon University, 7-7-1 Narashinodai, Funabashi, Chiba 274-8555, Japan
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.
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