- Phwang phap xa Ijr mit,: Mau HT de re
06i tuvng va phúóng phap nghien cúu
cúu
Nguyen lieu
Dau tam dung trong chiet xuat va phan lap: canh dau tam (Ramulus Mod albae) thu hai thang 2/2013 tai Da Let, Lam DOng. Cac mau nay duvc xac dinh ten khoa hoc la Morus alba L., Moraceae va lúu giir tai BO mon Dúóc lieu - Khoa Dúóc - Dai Hoc Y Duvc Tp. HO Chi Minh.
Dung m6i boa chat
Cac h6a chat dung chiet xuat nhú ethanol, dung trong phan lap nhú ethyl acetat, dung trong tinh khiet h6a cac chat nhú chloroform, ethyl acetat va cac dung mei thu6c thin khac dat tiou chuan tinh khiet dung trong kiem nghiem duvc lieụ
Dyng cu, thiet bi
PhO UV thu,c hien ten may quang ph6 Shimadzu UV-vis 1700. PhO MS thúc hien tren may Quattro Micro API (WATERS). Pho Ong hiking tip hat nhan (NMR) do tai phOng cau truc Vien Hoa hoc, Ha Nei va duvc thvc hien Wen may Bruker AV500 sir dung chat chuan not la tetramethylsilan (TMS). Mau dúac h6a tan trong DMSO-d6 hoac aceton-d6. Pho proton (1H-NMR)
duvc do a 500 MHz, pho carbon (13C-NMR)
duvc do 6' 125 MHz. DO dich chuyen hoa hoc duvc tinh theo thang ppm (TMS = 0) vai chuan la tin hieu cOa TMS. Cac hang so ghep (J) tinh
bang Hertz (Hz). HPLC Waters 2695, dau dO PDA 2996, bu,ac song phat hien 250 nm. Get sac k9 Restek Pinacle C16 (5 pm, 150 mm x 4,6 mm).
Phwang phap nghien cúu
Nguyen lieu cay dau tam dung trong chiet xuat va phan lap cac chat sau khi thu hai duvc phol kh6, xay thanh bet, ray qua ray cho met, duvc dOng nhat. Kiem tra va xac dinh nguyen lieu tiro:5'c khi thu,c hien nghien cúu chiet xuat phan lap.
Chiet xuat, phan lap
TO 9,5 kg bet canh dau tam, chiet xuat bang phuvng phap nghm kiet vai ethanol 96% thu duvc 356 g cao con toan phan. Cao con toan phan (cao dac) duvc ten vai da !pot, dun hOi lúu trong 30 phut 6' 50 — 60 °C vai ethyl acetat 3 len, gan 10c lay dich chiet. Gap cac dich chiet, thu hOi dung m6i thu duvc cao ethyl acetat g9i la cao A (cao dac). Phan cao con lai khong tan (cao B) duvc lay rieng. Cao A &roc phan tach thanh 10 phan doan bang sac k9 cot silicagel ca hat viva (Merck),dung moi rira giai la chloroform — ethyl aceat vai t9 le ethyl acetat tang dan. Phan doan 5 va 10 co tia, loc hong lay tua, tinh the va dat ten la MA-2 (31,5 mg). Phan dich tir phan doan 10 cho cac vet phat quang va tat quang Ian, thu hOi dung m6i duvc 5,54 g can (goi la A10). TÓ phan doan A10 bang k9 thuat sac k9 cot va dung m6i rira giai tuvng tu, thu duvc 7 phan doan nho han (10.1 den 10.7). Phan doan 10.2 co tua trang, ket tinh lai nhieu Ian trong chloroform thu duvc chat ket tinh trang, dat ten la MA-1 (285 mg). Phan doan 10.7 xuat hien chat ket tinh, goi la chat MA-4. Tinh the MA-4 vai ethyl acetat thu duvc khoang 1350 mg.