CC PHNG PHP TCH CHIT TERPENOID

3.1 Cc phng php chit tch

Cc hp cht thin nhin khi mi c tch thng di dng khng tinh khit,
v vy mun nghin cu, phn tch chng th trc tin phi tch chng thnh tng
cht ring bit di dng tng i tinh khit.
3.1.1. Phng php ho tan tong dung mi hu c
Phng php ho tan tong dung mi hu c c dng tch v tinh ch cc
cht hu c rn, da trn nguyn tc l cc cht rn khc nhau c ho tan khc
nhau trong cng mt dung mi. Dung mi thch hp la chn thng l dug
mi trong c ho tan ca cht rn cn tinh ch thay i nhiu theo nhit .
Bng cch to dung dch bo ho nhit cao ( thng l nhit si ca dung
mi), cc tp cht s dng kh tinh khit. Cng c khi mhi ta dng mt dung
mi c ho tan vo tp cht nhiu hn loi tp cht ra khi cht rn cn tinh
ch.
Dung mi thng l nc, ancol etylic, ancol metylic, axeton, axit axetic bng, ete,
benzen,cloroform, etylaxetat,.....hoc i khi l hn hp gia chng.
Khi cn tch hai hay nhiu cht cha tronhg hp vi nhng lng tng ng
nhau
3.1.2 Cc phng php chng ct
3.1.2.1 Chng ct n gin
Trong trng hp cn tinh ch mt cht lng, tch n ra khi tp cht rn khng
bay hi, ta ch cn tin hnh chng ct thng (chng ct n gin), ngha l
chuyn chng sang pha hi trong mt bnh ct c nhnh ri ngng t hi ca n
bng ng sinh hn vo mt bnh hng khc. Thng c p dng tinh ch cc
cht th. Trong ho hu c, thng c p dng ui dung mi tch tinh du.
3.1.2.2 Chng ct phn on
Phng php chng ct phn on dng tch hai hay nhiu cht lng c nhit
si khc nhau tan ln hon ton trong nhau, da trn nguyn tc c s phn b
khc nhau v thnh phn cc cu t gia pha lng v pha hi trng thi cn bng
( cng nhit ). Nh vy, bng cch lp i lp li nhiu ln qu trnh bay hingng t; bay hi- ngng t lita dn dn c th thu c cu t A c nhit

si thp hn dng gn tinh khit. V vy ngi ta dng phng php tinh luyn
bng cch lp trn bnh chng ct mt ct cao c nhiu a (ct Vigr) gip cho
vic ti to qu trnh bay hi ngng t trn. Nh vy cht lng A d bay hi dn
dn thot ln trn, trng thi ngy cng tinh khit, cn cht lng B c nhit si
cao hn, ngng t tr li bnh chng.
C th ngi ta dng loi ct lp y cc mnh hoc ng thu tinh hay cc mnh
s thay cho ct Vigr v hiu qu ca ct c tnh bng s a l thuyt.
3.1.2.3 Chng ct di p sut thp
Khi cn chng ct mt cht lng d phn hu nhit cao, ngi ta phi dng
phng php chng ct di p sut thp, tc l dng bm ht gim p sut trn
b mt cht lng. V cht lng s si khi p sut ring phn t n p sut kh
quyn, nn bng cch ny ngi ta c th gim c nhit si ca n mt cch
ng k, trnh c hin tng phn hu hay chy n. Nh phng trnh
Claparon- Clausius, ngi ta c th tnh c s ph thuc ca p sut hi ca mt
cht vo nhit . Tuy nhin, c th p dng quy lut thc nghim gn ng nh
sau: Khi p sut kh quyn trn b mt cht lng gim i mt na, th nhit si
ca n h thp i khong 150C.
3.1.2.4 Chng ct li cun hi nc
Ta c th tinh ch mt cht lng khng ho tan trong nc bng phng php
chng ct li cun hi nc h im si ca n. Phng php ny da trn
nguyn tc: Khi hai hay nhiu cht lng khng trn ln vi nhau nm trong mt
hn hp, p sut chung ca chng bng tng p sut ring phn p1 + p2, ngha l
n lun lun ln hn p sut ring phn ca bt k cu t no. Do nhit si
ca hn hp s thp hn nhit si ca cu t c nhit si thp nht. T l hi
ct sang bnh ngng (v s mol) s bng t l p sut hi ring phn ca chng
nhit si ca hn hp. Nh vy ta c th tnh ton c lng nc cn thit

li cun ht cht cn tinh ch.

Sau khi dng phng php chng ct li cun hi nc, thng ta phi chit
tch cc cht cn tinh ch ra khi nc bng mt dung mi thch hp, ri li tin
hnh chng ct phn on tch dung mi. Cui cng chng ct ly tinh khit
bng bnh chng ct c gn nhit k di p sut thp, vi s kim tra nhit ca
cht cn tinh ch.
3.1.3 Phng php chit
3.1.3.1 Gii thiu chung
Chit l dng dung mi thch hp c kh nng ho tan cht ang cn tch v tinh
ch tch cht ra khi mi trng rn hoc lng khc. Thng ngi ta dng
mt dung mi si thp v t tan trong nc (v cc cht hu c cn tinh ch thng
t tan trong nc), cht s chuyn phn ln ln dung mi v ta c th dng phu
tch ring dung dch thu c ra khi nc.

Bng cch lp i lp li vic chit mt s ln, ta c th tch hon ton cht cn tinh
ch vo dung mi chn, sau ct loi dung mi v ct ly tinh khit nhit
v p sut thch hp.
Ngi ta cng thng chit mt cht t hn hp rn bng mt dung mi hoc hn
hp dung mi vi mt dng c chuyn dng c bit gi l bnh chit Soxhlet.
Dung mi c un nng, cho bay hi lin tc chy vo bnh cha hn hp cn
thit tch (thng gi trong giy lc), n s ho tan cht rn cn tinh ch v nh
mt ng xiphng, dung dch chy xung bnh cu bn di, dugn mi nguyn cht
li tip tc c ct ln. Phng php ny tit kim c dung mi v hiu qu
tng i cao.
3.1.3.2. Chit Soxhlet
Chit soxhlet l mt kiu chit lin tc c bit thc hin nh mt trang b ring
ca n. Kiu chit ny cng nh kiu chit lng- lng nn v bn cht ca s chit
vn l nh lut phn b trong hai pha khng trn vo nhau. Song y pha mu l
trng thi lng, bt, hoc dng mnh hoc dng l. Cn dung mi chit (cht hu
c) l dng lng.

3.2 Tch chit monoterpenoid v sesquiterpenoid

Hu ht cc monoterpenoid v sesquiterpenoid c nhiu trong tinh du ca cc loi

thc vt.
Phng php c in tch cc thnh phn c trong tinh du l tin hnh ct phn
on p sut gim hoc p sut thng. Ct ct phn on phi c s lng a
tch nhiu. Cc hydrocacbon bo v monoterpen n gin s bc hi trc, tip
n l monoterpen c nhm Oxi, ri n cc hp cht thm v cui cng l cc
sesquiterpen. Phn cn li trong bnh s l cc sn phm polyme, diterpen v hp
cht azulen.
Sc k ct cng l mt phng php dng tch cc terpenoid c trong tinh du

Tch methol
Tch citral
Tch Eugenol
Tch cedrol
Tch methyl chavicol

3.3. Tch chit cc hp cht lacton terpenoid

Trong cc terpenoid cc hp cht c vng lacton m c bit l sesquiterpen lacton
chim mt v tr quan trng v nhiu ng dng ca chng trong y hc cng nh
nng nghip. C th: chng c tc dng c t bo, khng ung th, khng trng,
dit cn trng v dit nm.
Sesquiterpen lacton phn b ch yu trong cc cy thuc tho v cy bi. c bit
tp trung trong h Aeteraceae. Trong cy chng tp trung ch yu trong l, hoa, ni
chung l cc b phn trn mt t.
Cc sesquiterpen lacton l cht phn cc trung bnh, chng tan tt trong CHCl 3 v
dietyl ete, tan t hn trong Metanol v etanol lnh nhng tan nhiu nng. Da
vo tnh cht ny, ngi ta chit sesquiterpen lacton theo cc cch sau:

Chit bng CHCl3

Chit bng cn v nc nng
Chit bng cn (EtOH hoc MeOH)
Chit bng dung dch kim nng.