Daiso Co., Ltd.) packed with water. The
column was washed with water (5 l) and eluted with 42% aqueous
acetonitrile containing 0.1% TFA (4 l). The active fraction (2–3 l) was
diluted with an equal volume of water and then loaded into a
Daisogel SP-120-ODS-B column (15/30 mm, Daiso Co., Ltd.) packed
with water. The column was washed with water (5 l) and eluted with
40% aqueous acetonitrile containing 0.1% TFA (5 l). The active
fraction (1.5–3.5 l) was diluted with an equal volume of water and
then loaded into a Daisogel SP-120-ODS-B column (15/30 mm, 0.2 l;
Daiso Co., Ltd.) packed with water. The column was washed with
water (1 l) and eluted with methanol (0.2 l).