옥수수수염에 함유되어 있는 maysin 및 유사 flavonoid 물질의 분리 및 정제법을 확립하여 신품종 육성의 기초적인 자료를 제공하고자 본 시험을 수행하였으며 얻어진 결과를 요약하면 다음과 같다. 1. Preparative C18 컬럼에서 10% MeOH에 용출된 물질은 neochlorogenic acid, chlorogenic acid 및 4-caffeoylquinic acid였으며 30% MeOH로 용출된 물질은 rhamnosyl isoorientin이었고 maysin은 50%의 MeOH에서 용출되었다. 2. Silicic acid 컬럼으로 maysin 조추출물의 1차 정제시 100% ethyl acetate 500m 로 컬럼에 흡착되어 있는 maysin을 용출시켰으며, 이때 수거된 maysin의 순도는 75% 이상에 해당하였고, C18 컬럼(12 43")으로 maysin의 2차 정제시 maysin의 순도는 95% 이상에 달하였다. 3. FAB-MS에 의한 maysin의 분자량은 577M＋H m/z이고, fragmentation으로 보아 431M＋H m/z은 rhamnose에 해당하였고, 1 H 및 13C NMR에 의한 spectrum을 확인한 결과 분리한 물질이 maysin임을 확인할 수 있었다. 있었다.

This study was carried out to isolate and identify the maysin and related flavonoid analogues in corn silks. Silks were covered with silk bag to prevent pollination and were sampled at 3-5 days after silking. The silks were filled with 100% MeOH and stored at 0~circC until analysis. The MeOH extracts of corn silks were filtered and concentrated at 35-40~circC . The CH2 Cl2 was added on the concentrated aqueous solution to remove the chlorophyll and lipids. The Cis open column (25mm~times 54 cm) was washed and activated with serial treatment of 500m~ell of 100% MeOH(twice)longrightarrow75% MeOH longrightarrow50% MeOHlongrightarrow30% MeOHlongrightarrow100% H2 O(2 times). The concentrated aqueous solution was applied to the C18 column and washed with H2O several times to remove the sugars and water soluble pigments. Neochlorogenic acid, chlorogenic acid and 4-caffeoylquinic acid were eluted with 10% MeOH, and rhamosyl isoorientin was eluted with 30% MeOH, but maysin was eluted with 50% MeOH from the C18 open column. Collected fractions were analyzed with HPLC by using revers-phase Ultras-phere C18 column (4.6~times 250mm, 5~mu~textrmm ) and H2 O (10% MeOH containing 0.1% H3 PO4 )/MeOH (100% MeOH containing 0.1% H3 PO4 ) linear gradient from 20% to 90% MeOH for 35 minutes, a flow rate of 1 m~ell /min and detection at 340nm. The selected fractions were concentrated and applied to the silicic acid column. Maysin was eluted with 500m~ell of 100% ethyl acetate from the silicic acid column for the first purification, and the purity of collected fractions was about 75%, but the purity from the second purification with the Cis column (1/2 ~times 43") was greater than 95%. FAB-MS spectral data was obtained with VG7O-VSEQ VG analytical fast atom bombardment mass (UK). 1 H-NMR and 13 C-NMR data were obtained with Bruker DPX 400 MHz NMR spectrometers (German) in DMSO-d6 at 400 and 100 MHz,

• 김선림
• Maurice E. Snook
• 김이훈
• 박철호