It has been known that the seed of "Moroheiya"(Corchorus olitorius L.) contains cardiac glycosides such as Strophanthidin (SP) as an aglycon. Using trimethylsilyl (TMS) derivatization and GC/MS analysis, a simultaneous method for the determination of SP and Digitoxigenin (DG) in "Moroheiya" was developed. The condition for TMS derivatization of SP and DG was examined using commercially available standard reagents. Each reagent was treated with a mixture of pyridine, N, O-bis (trimethylsilyl)-acetamide, trimethylsilylimidazole and trimethylchlorosilane and analyzed by GC/MS. Their mass spectra demonstrated the formation of the completely and partially derivatized TMS ethers, SP (TMS)
4, SP (TMS)
3, SP (TMS)
2, DG (TMS)
3 and DG (TMS)
2. The complete derivatization from SP to SP (TMS)
4 and DG to DG (TMS)
3 required the reaction for about 20h at 100°C. SP and DG in C. olitorius seeds and processed "Moroheiya" foods were prepared as follows; "Moroheiya" sample was hydrolyzed in a 1% sulfuric acid-methanol (1:1, v/v), and then the resulting hydrolyzate was extracted with dichloromethane. The extract was dried up and derivatized for 20h at 100°C. The resulting derivatives, SP (TMS)
4 and DG (TMS)
3 were determined by GC/SIM (selected ion monitoring). The mass spectra of those derivatives were not significantly affected by interfering components. Thus, this method is confirmed to be very useful for qualitative and quantitative analysis of SP and DG in "Moroheiya" samples. The detection limits of SP and DG were 5mg/kg and 1mg/kg, respectively. By the present method, 5.9-6.2g/kg of SP and 0.15-0.24g/kg of DG were detected in C. olitorius seeds, while neither SP nor DG was detected in processed "Moroheiya" foods.
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