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2- BT MA HONG (100ng/1kg)

un ha cht
DD Toluen, a xt, dd NAOH (xt n da)
3- thuc ho Recotus

L thuyt ha hc cn ghi nh]


Phng php tch v tinh ch mt s hp cht
hu c
Phng php vt l (Phn I)
a)Phng php kt tinh li :
--y l phng php quan trng nht tinh
ch cht rn .Phng php kt tinh li da trn
s khc nhau r rt v tan ca cc cht
trong mt dung mi (hay hn hp cc dung

mi ) cc nhit khc nhau ,hoc c s


khc nhau v tan gia cht chnh v tp
cht cng mt nhit
--Thng ta chn dung mi (hay hn hp dung
mi ) ha tan cht cn kt tinh khi un
nng v t ha tan cht khi lm lnh .Khi
lm lnh dung dch bo ha ,cht kt tinh lng
xung dng tinh th cn tp cht li trong
dung dch (nu tp cht khng tan khi un
nng th cn lc b ri lm lnh dung dch bo
ha)
b)Phng php chit
--Chit dng tch cc cht thng l cht
lng ra khi hn hp lng khng ng nht
(phn lp)
--Ty theo bn cht ca cht c chit v mi
trng chng ang tn ti m ta chn dung
mi thch hp chit
c)phng php lm kh
--Cht rn sau khi kt tinh li ,cht lng sau khi
chit hoc cht kh thu c sau phn ng
iu ch thng ln vt nc hoc mt lng
nh dung mi.Vic loi b dung mi hoc nc
t cc cht trn c gi l lm kh
-- lm kh ngi ta dng cht hp th nc

(cht lm kh) hoc cho bay hi nc hay cho


bay hi dung mi
--Quan trng nht l lm kh nc nh cht
lm kh .Cht lm kh phi tha mn cc iu
in :C kh nng hp th nc cao,c tc
dng lm kh nhanh ,khng tng tc ha hc
vi cht c lm kh ,r tin
C th chia cht lm kh thnh 3 nhm chnh
.Cc cht c tnh axit:H2SO4 c ,P2O5,..
.Cc cht c tnh bazo:NaOH rn ,KOH
rn ,K2CO3 khan ,CaO khan
.Cc cht trung tnh:MgSO4khan ,Na2SO4
khan,CuSO4 khan,...
d) Phng php thng hoa
--Thng hoa l s chuyn cht t trng thi rn
sang trng thi hi m khng qua trng thi
lng .Ngc li s ngng t cht t trng thi
hi v trng thi rn gi l s chng thng hoa
--Nguyn nhn ca s thng hoa l do p sut
hi ca cht rn tng theo nhit nn khi
un nng n nhit m p sut hi ca cht
rn bng p sut bn ngoi th cht thng
hoa .Da vo tnh cht ny tinh ch cc
cht rn c p sut hi kh ln nhit thp
hn nhit nng chy ca chng ti p sut

thng ,v d tinh th iot,axit


benzoic ,naptalen,quinon ...i vi nhng cht
t bay hi hoc khng thng hoa p sut
thng hoc thng hoa rt chm th tin hnh
p sut thp
Herba Ephedrae
end of page
1. nh ngha dc liu
1.

B phn trn mt t phi hoc sy kh ca cy tho


Ma hong (Ephedra sinica Staff.), Mc tc ma hong
(Ephedra equisetina Bunge.), Trung gian ma hong
(Ephedra intermediaSchrenk. et C. A. Meyer); h Ma
hong (Ephedraceae).

2. c im thc vt
M t
Tho ma hong: L nhng nhnh hnh tr trn, ng knh 1 - 2 mm, t
phn nhnh. Mt ngoi mu xanh l cy nht n xanh vng, c nhiu
rnh dc, hi rp tay. Thn chia thnh nhiu t v dng r, mi dng di
2,5 - 3 cm; l hnh vy nh, di 3 - 4 mm, mc i t khi mc vng, pha
trn u l nhn v cong. Th cht gin, d gy, vt b c x, rut c mu
nu . Mi thm nh. V hi ng, cht.
Mc tc ma hong: Thn c ng knh 1 - 1,5 mm, khng rp tay,
thng phn nhnh nhiu. Dng di 1 - 3 cm. L l nhng vy hnh
tam gic, di 1 - 2 mm, mu trng xm, u l khng cun li; rut c
mu nu n nu en. Trung gian ma hong: ng knh 1,5 - 3
mm, thng phn nhnh, rp tay, dng di 2 - 6 cm. L l vy di 2 - 3
mm, thng umc vng, u l nhn (V thuc Ma hong).

Dc phm
Tn IUPAC h thng
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2.

Thnh phn
ho hc

metham
phetami
ne
(meth) l
(

3.

)2(methy
Alc eph lamino
aloi edri )-1d: n* phenyl
propan
-1-ol
nore
phe
drin
met
hyle
phe
drin.
flav
ono
id
tani
n
tinh
du
,

N-methyl-1-phenylpropan-2-amine
Nhn dng
S CAS

537-46-2

M ATC

N06BA03

PubChem

1206

DrugBank

DB01577

D liu ha cht
Cng thc

C10H15N

Phn t gam

149.2337 g/mol

SMILES

tm
trong eMolecules,PubChem

ng ngha

Desoxyephedrine
Methamfetamine
Pervitin
Anadrex
Methedrine
Methylamphetamine
Syndrox
Desoxyn
Pervitin

D liu dc ng lc hc
Hiu lc sinh hc

62.7% oral; 79% nasal;


90.3% smoked; 99%
rectally; 100% IV

Chuyn ha

Hepatic

Bn thi

912 gi

Bi tit

Renal

Lu tr liu
Phm tr thai sn

C(US)

Tnh trng php l

Controlled (S8)
(AU)Schedule

acid hu c.
.
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4. Kim nghim
Vi phu
Tho Ma hong: Biu b ngon ngoo, c lp cutin dy, l kh thng
nhng ch lm. Ti cc gc li nm st biu b c nhng b si thnh rt
dy khng ho g. Vng m mm v kh rng, c nhng b si nh nm
ri rc. Tr b c hnh un khc v di nhng gc li c nhng b si.
Vng libe-g gm 8 - 15 b, libe pha ngoi, g pha trong (mch g
cha phn ho). M mm, rut cha nhng khi c mu nm ri rc, i
khi c nhng m si. (Vi phu thn ma hong)
Mc tc ma hong: C 8 - 10 b si vng tr b. Tng sinh libe - g l
mt vng lin tc. Khng c si trong rut. Trung gian ma hong: C 12 15 b si nm vng tr b. Tng sinh libe - g c dng tam gic. Si
trong m mm rut nm ri rc, ring l hay thnh b.
Soi bt
Mu vng xanh hay vng nu. Soi knh hin vi thy: Mnh biu b thn
mang l kh, lp cutin c u li. Si di c vch dy nm ring l hay chm
thnh b. Mnh m mm gm c nhng t bo hnh ch nht, vch mng.
Khi mu cam, nu, nu en. Mnh mch vch c kch thc nh.(Mt s
c im bt Ma hong)
nh tnh
A. Bt dc liu, chit bng dung dch acid hydrocloric 5% nhit si,
Lc. Chuyn dch lc vo mt bnh gn, kim ho bng amoni hydroxyd
m c, ri chit bng cloroform. Gn dch cloroform vo hai ng nghim.
ng 1 thm dung dch ng (II) clorid kim (TT) v carbon disulfid (TT),
mi loi 5 git, lc u v yn, lp cloroform c mu vng m. ng 2
dng lm ng kim chng, thm 5 git cloroform (TT) thay v carbon
disulfid, lc u v yn, lp cloroform khng c mu hay c mu vng
rt nht.

B. Phng php sc k lp mng (Sc k lp mng).


S dng bn mng Silicagel G hot ho 1100C trong 30 pht, h dung
mi khai trin: cloroform - methanol-amoni hydroxyd m c (20: 5: 0,5).
Dung dch th: Bt dc liu, kim ho bng amoni hydroxyd m c v
chit bng cloroform, un hi lu 1 gi, lc. Bc hi dch lc ti cn, thm
methanol vo cn ri khuy u. Lc, c dung dch th.
Dung dch i chiu: Ho tan mt lng ephedrin chun trong methanol
(TT) c dung dch c nng 1 mg/ml.
Cch tin hnh: Chm ring bit ln bn mng cc dung dch trn, trin
khai sc k xong, kh bn mng nhit phng, phun dung dch
ninhydrin (TT) v sy 105oC khong 5 pht. Trn sc k ca dung
dch th phi c vt cng mu sc v gi tr Rf vi vt ephedrin trn sc k
ca dung dch i chiu.
C th s dng sc k lp mng hiu nng cao nh tnh Ma hong:
Chit dc liu bng MeOH. S dng bn mng silicagen, trin khai bng
h dung mi v quan st = 366nm(Sc k dch chit cc dc
liu vt 2).
nh lng
Cn chnh xc mt lng bt dc liu kim ho bng amoni hyroxyd
m c, cho vo bnh Soxhlet, thm ethanol v ether. yn 24 gi,
thm ether v un hi lu trn cch thu cho n khi ht alcaloid. Chuyn
dch chit vo mt bnh gn, ra bnh chit bng mt lng nh ether. Lc
dch chit vi dung dch acid hydrocloric 0,5 M nhiu ln. Gp ht dch acid
li, kim ho bng dung dch natri hydroxyd 40%, bo ho bng natri
clorid, li chit vi ether nhiu ln. Gp cc dch ether li, ra 3 ln mi
ln 5 ml dung dch natri clorid bo ho. Gp cc nc ra li v lc vi 10
ml ether. Gp ht cc dch ether li, thm chnh xc 30 ml dung dch acid
sulfuric 0,01 M, lc u, yn lp acid trong bnh gn cho phn lp; ly
ring lp acid cho vo bnh nn, ra dch ether bng nc. Gp nc ra
vo bnh nn ng acid trn, un cch thu ui ht ether v ngui,
chun acid tha bng dung dch natri hydroxyd 0,02 M, dng 2 git
methyl lm cht ch th mu. 1 ml acid sulfuric 0,01 M tng ng vi

3,305 mg ephedrin (C10H15NO). Dc liu phi cha khng di 0,8%


alcaloid ton phn tnh theo ephedrin C10H15NO.
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5. Tc dng v cng dng
Pht hn, tn hn, tuyn ph, bnh suyn, li thu, tiu thng. Ch tr:
Cm mo phong hn, ngc tc, ho suyn, phong thy ph thng,
hen ph qun.
Mt Ma hong: Nhun ph ngng ho; thng dng trong trng hp
biu chng gii, kh suyn ho.
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6. Ghi ch
Ch bin
Thu hoch vo ma thu, khi thn cn hi xanh, ct v, phi kh, b
li thnh tng b.
Bo ch
Ma hong: B phn gc thn ho g, r cn st v tp cht, ct on,
phi kh.
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1- THUC DENAUSAL
* 4000 vin + 2000ml H2O/24h ----- > thuc tan + 5000ml xng thm (butin) khuy u.
* cho tip 300-400g (gram) xt xc u 10 pht ---> lng cn
* gn ly dung dch --- > lc + 10.000ml H2O + 10 ml ( cc ) axit clohydric - un-- > hn
hp st st
* Axeton (pht pho , hoc cn I t)

#xt trong cc phn ng trn ng vai tr cht lm kh


* 40 vin + 20 ml H2O/24h ----- > thuc tan + 50 ml xng thm (butin) khuy u.
* cho tip 3-4g (gram) xt xc u 10 pht ---> lng cn
* gn ly dung dch --- > lc + 100 ml H2O +0.1 cc axit clohydric - un-- > hn hp st st
* Axeton (pht pho , hoc cn I t)

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