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Optimalizace GC/MS metody stanovení silyl derivátů lignanů
 BEDNÁŘ, Jan
The main goal of this work was optimization of GC-MS method for the analysis of lignans trimethylsilyl (TMSi-) derivatives of two model compounds hydroxymatairesinol(HMR) and enterolactone (ENTL). It included validation of GC-MS metod for TMSiHMR and TMSi-ENTL, comparison of chosen derivatization reagents and verification of time stability for TMSi-HMR. It was shown that TMSi-HMR and TMSi-ENTL provide a nonlinear calibration curve. Second order polynomial curve gave the best fitting and was used for method validation. N-Methyl-N-(trimethylsilyl)trifluoroacetamide activated I and II (Sigma Aldrcih) were selected as the best choice for simultaneous derivatization for HMR and ENTL mixture. Room temperature was confirmed to be appropriat for 3 days storage of TMSi-HMR. Also it was shown that storage at -80 °C preserve the lignan samples for at least 90 days storage.
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