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V Ngc L, Nhng Cy Tinh Du Vit Nam. Nxb Khoa hc v K thut (1996) 3. L Vn ng, Chuyn Mt S Hp Cht Thin Nhin. Nxb i hc Quc gia Thnh ph H Ch Minh (2005)
4. Nguyn Ngc Sng, Alkaloid. i hc Khoa Hc T nhin- Thnh ph H Ch Minh 5. B.s Durt Randerath-Dunnschicht-Choomatographie Vin khoa hc hu c thuc trng i hc k thut Darmstadt (c). 6. R.H. Thomson, The Chemistry of Natural Products. Chapman & Hall (2007)
***Thin nhin cha rt nhiu cht hay hp cht phuc vu cho s tn tai va pht trin cua con ngi.
Cy du tm. Ton b cy du tm v qu u cho ta nhiu cht tt, nh: triterpen, protein, gluxit, flavonoit, cumarin, cc vitamin B, C, D, caroten, cc a-xit hu c khc. Trong cy ( l v ht c hm lng cao nht) c cha nhiu ancaloit (hm lng ton phn t 0,2-0,5%), chu yu l scopolamin, cn c hyoscyamin, atropin v cc saponin, flavonoit, tanin... vi s lng khng ng k.
I. KHI QUT V HP CHT THIN NHIN II. PHNG PHP LY TRCH II.1. LY TRCH L G? II.2. NGUYN TC LY TRCH II.3. CC PHNG PHP LY TRCH III. PHNG PHP LY TRCH MT S HP CHT THIN NHIN IN HNH III.1. ANCALOIT
III.2. STEROL III.3. CUMARIN III.4. TINH DU
I. KHI QUT V HP CHT THIN NHIN V mt phn loi ha hc, hp cht t nhin c sp xp theo cc nhm chc c bn: - Hidratcacbon (monosaccarit, oligosaccarit, polisaccarit). - Lipid v axit bo. - Axit amin (protein v phi protein).- Baz amin (ancaloit, amin).
- Axit hu c. - Tecpenoid (mono, sesqui, i, tritecpen, carotenoid, steroid,). - Hp cht phenol (Flavonoid, tannin, lignin, quinon,).
- Glycozit
Ly trch (chit) l phng php dung mt dung mi (n hay hn hp) tch ly mt cht hay mt nhm cc cht t hn hp cn nghin cu. Trng hp thng gp nht l s chit hot cht t dung dch nc vo dung mi hu c. Dung mi c t trng nh hn s lp trn nh: eter, benzene, cc hyrocacbua, dung mi c t trng lp hn s lp di nh: chloroform, tetracloriccacbon, icloetan, khi trn ln 2 pha nc v dung mi hu c vi nhau
pha kia nhng v c bn mt pha vn l nc v pha kia vn l dung mi hu c. Khi lc 2 pha li vi nhau, th tch 2 pha khi lc khng bng ng nh th tch trc khi lc. Tuy nhin cho n gin, gi thit rng th tch ca pha l khng i khi lc. Ly trch nhm mc ch iu ch hay phn tch.
Phng php c in li trch mt hp cht thin nhin l dung mt dy dung mi bt u t khng phn cc n phn cc mnh li trch, phn on cc hp cht ra khi hp cht thin nhin. .V d :
Dy dung mi: ete du, ete, clorofom, cn v cui cng l nc
Cch li trch thng dng l li trch nng bng my li trch lin tc hoc li trch hi lu. Sau mi ln li trch vi mt loi dung mi cn lm kh hp cht thin nhin ri mi tip tc li trch vi loi dung mi tip theo. Mi phn on li trch, ct thu hi dung mi v tin hnh phn tch ring
Da vo tnh phn cc ca dung mi v ca cc nhm hp cht ta c th d on s c mt ca cc cht trong mi phn on li trch. - Trong phn on li trch ete v ete du s c cc hidrocacbua bo hoc thm, cc thnh phn ca tinh du nh monotecpen, cc cht khng phn cc nh cht bo,carotene,cc sterol, cc cht mu thc vt,clorophyl.
- Trong dch li trch clorofom s c mt sesquiterpen, diterpen, cumarin, quinon, cc aglycol do glycozit thy phn to ra, mt s ancaloit baz yu, Trong dch li trch nc s c cc glycozit, tannin, cc ng, cc hp cht hidrat cacbon phn t va pectin, cc protein thc vt v mui v c.
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- Khi cn li trch ly ton b thnh phn trong hp cht thin nhin th dung mi thch hp nht l cn 80%. Cn, nht l metanola c xem l dung mi vn nng. N ha tan c cc cht khng phn cc ng thi cng c kh nng to dy ni hidro vi cc nhm phn cc khc
Dch ly trch cn em bc hi dung mi s c cao ton phn cha hu ht hp cht thin nhin. Khi cn tch phn on cc hp cht trong cao th s dng mt dy dung mi khng ha ln vi nc v c phn cc t yu n mnh. V d dy dung mi: ete du, ete, clorofom, etila axetat, butanola.
II.2. NGUYN TC LY TRCH (tt) Cch ly trch: C hai cch ly trch : ly trch nhit thng v ly trch nng. Mi cch ly trch c dung mi v thit b ring. - Hai cch ly trch thng thng nhit thng l ngm kit v ngm phn on. Phng php ngm kit cho kt qu tt hn v ly trch c nhiu hot cht v t tn dung mi, nht l khi p dng cch ly trch ngm kit ngc dng. - Ly trch nng: nu dung mi l cc cht bay hi th p dng cch ly trch lin tc v ly trch hi lu. Nu dung mi l nc th sc hoc hm phn on.
Dng c ly trch lin tc thng thng l bnh Soxhlet. C th t lp ly dng c ly trch lin tc. Nu ly trch nng hi lu th nn ly trch phn on t nht l hai ln ly trch ht hot cht.
Tnh phn cc ca hp cht t nhin c quan h n vn li trch hp cht thin nhin. Mt yu t khc cng c nh hng n vn li trch l cc enzim vn lun c mt trong cy. Trong qu trnh ch bin, li trch nu khng khng ch c hot tnh ca men th cc glicozit c th b thy phn mt phn hoc ton phn lm thay i tnh phn cc, do thay i ha tan ca hp cht i vi dung mi.
Dung mi dung li trch cc hp cht khi cc hp cht thin nhin rt a dng v thay i ty theo bn cht ca mi loi hp cht thin nhin. C s la chn mt dung mi li trch l tnh phn cc ca hp cht cha trong hp cht thin nhin v ca dung mi
Ly trch n (Chit mt ln): thng cho hiu sut thp. Ly trch lp (chit nhiu ln): nu h s phn b khng ln trch mt ln th phi trch thm nhiu ln. Ngha l sau khi chit mt ln, trong dung dch cn li mt lng cht tan ng k th thng ngi ta thm mt lng dung mi chit mi v chit mt hay nhiu ln na. Hiu sut cao hn hiu sut chit n nhng tn dung mi, thi gian v cng sut.
Ly trch ngc dng: Phng php ny da trn nguyn tc cho dung mi ly trch vo dung dch cn ly trch chy ngc chiu nhau. Hai pha tip xc cht ch, pha trn v di chuyn ngc chiu nhau. y l mt qu trnh lin tc.
Mc tiu ca s phn chia ngc dng l tch hai hay nhiu cht tan ra bng mt lot s phn chia gia hai pha lng-lng. tm hiu c s l thuyt ca phng php ny v n gin ha, hy hnh dung s li trch c thc hin mt cch gin on qua nhiu bc.
Trong cy, ancaloit tn ti di dng mui ca cc axits hu c nhng mt s kt hp vi tannin (nht l nhng cy c nhiu tannin) v vy i vi hp cht thin nhin c nhiu tannin th cn dung dung mi c phn cc mnh hn hoc chit nng tch cc ancaloit ra khi tannin v ha tan vo dung mi
Mt s ancaloit l cc este nh: Atropin, cocain, heliotrin c th b thy phn trong qu trnh ly trch nn rt hn ch s dng nhit cao. Ngc li, mt s ancaloit tn ti trong cy di dng glicozit(glicoancaloit) nh solamacgin, solasonin trong cc loi solanum. ly trch cc ancaloit ny cn c giai on thy phn
III.1. ANCALOIT(tt)
Ni chung ancaloit l mt cht tng i bn vng so vi nhiu hp cht t nhin khc. Nhng mt s hp cht thuc dn xut Indol rt d b hy hoc bin cht bi nh sang, v cc tc nhn oxi ha kh khc nn cn ch khng ch cc yu t c th lm hng ancaloit trong qu trnh ly trch trong kh quyn.
III.1. ANCALOIT(tt)
Ancaloit c th ly trch t hp cht thin nhin kh tn bt. hn ch bt kh khn trong qu trnh ly trch i vi hp cht tin nhin cha nhiu cht bo, cht mu nn c giai on loi tp s b.
i a s ancaloit l cht kt tinh khng mu v c im chy xc nh, ch c mt s ancaloit c mu vng (becberin, palmatin,) c th li dng mu ny theo di chng trong qu trnh ly trch
III.1. ANCALOIT(tt)
C 2 cch - Ngm bt hp cht thin nhin vi ete du hoc ete trong vi gi n mt ngy - Chit lin tc bng Soxhlet hoc hi lu vi ete du, 1 n 2 gi. Bt loi tp xong, kh t nhin.
Cy Vang ng
Cy Ba Gac
III.2. STEROL
Sterol l cht khng phn cc, rt t tan trong nc tan trong du bo, carotene, letcitin. Tan trong cc dung mikhng phn cc nh: ete du, ete, bezen, CHCl3 nn cc cht ny thng c dung lm dung mi ly trch chng. Ngoi ra cn c th ly trch sterol bi cn (dng glycozit).
III.3. CUMARIN
Cumarin l cht phn cc yu nn a s tan trong ete du v ete etylic. Nhiu trng hp c th thu c tinh th cumarin ngay trong dung dch ete hoc ete du. Do c mt nhm lacton, mt s cumarin c thm OH phenol nn chng tan c trong kim nng. V vy c th ly trch chng bng dung dch kim nng. Dch ly trch kim em axt ho s thu c kt ta cumarin c th tinh ch cumarin bng cch thng hoa nhng ch p dng i vi cc hp cht bn vng vi nhit
III.4. TINH DU
Tinh du c nhiu b phn khc nhau trong cy: l, hoa, thn, r, qunguyn liu ly trch tinh du c th ti hoc kh, nhng c iu kin th dung ti tt hn v thnh phn khng b phn hy hoc hao ht trong qu trnh lm kh C nhiu phng php ly trch tinh du: ct vi nc, ly trch bng dung mi hoc p trong phng nghin cu, ly trch lng nh, c th dung bnh cu v ng sinh hn thy tinh c ni un nc nng st nc nng.