him im ng m K c ph d
Nng, 7/2011
1
Kim nghim dc phm
Kim nghim dc phm
Nhm 4
Chng 1: Tng quan
1 3 2
Gii thiu v Clopheniramin Cc phng php xc nh
Nng, 7/2011
2
TNG QUAN
Kim nghim dc phm
Nhm 4
Tn chung quc t:Chlorpheniramine. L vin nn cha clorpheniramin
maleat. Loi thuc: Thuc i khng th th H1 histamin Cng thc phn t:
C16H19ClN2.C4H4O4NMe2 H N COOH
.
Cl
COOH
Dng thuc v hm lng:Vin nn: 4 mg, 8 mg, 12 mg. Hm lng: 90,0 n
110,0% so vi hm lng ghi trn nhn. Nng, 7/2011
Clorpheniramin maleat
3
TNG QUAN
Kim nghim dc phm
Nhm 4 Tnh cht: Vin nn mu trng hoc vng
nht. Tc dng dc l: C rt t tc dng an thn, tc dng ph l chng tit
acetylcholine.. Tc dng khng histamin thng qua phong b cnh tranh cc
th th H1 ca cc t bo tc ng. Tc dng ng hc: Hp thu tt khi ung v xut
hin trong huyt tng trong vng 30 - 60 pht. Chuyn ha nhanh v nhiu.
Thuc c bi tit ch yu qua nc tiu. S bi tit ph thuc vo pH v lu lng nc
tiu. Nng, 7/2011 4
TNG QUAN
Kim nghim dc phm
Nhm 4 Cng dng:Cha vim mi d ng ma v quanh nm vi nhng triu chng
khc nhau nh: my ay, vim mi vn mch do histamin, vim kt mc d ng, vim
da tip xc, ph mch, ph Quincke, d ng thc n, phn ng huyt thanh, cn
trng t, nga ngi bnh b si hoc thy u. Phi hp trong mt s ch phm bn trn
th trng iu tr triu chng ho v cm lnh. Bo qun: ni kh, mt, trnh nh
sng.
Nng, 7/2011
5
TNG QUAN
Kim nghim dc phm
Nhm 4
2 phng php
Nng, 7/2011
6
TNG QUAN
Kim nghim dc phm
Nhm 4Nguyn tcl mt k thut sc k c dng tch cc cht trong hn hp. Bao
gm pha tnh l mt lp mng cc cht hp ph, thng l silicagel, aluminium
oxit, hoc xenlulozo c ph trn mt mt phng cht tr; pha ng bao gm dung
dch cn phn tch c ha tan trong mt dung mi thch hp v c ht ln bn sc k
bi mao dn, tch dung dch th nghim da trn tnh phn cc ca cc thnh phn
trong dung dch. Xt nghim tinh khit ca cc ha cht phng x trong dc
khoa Xc nh cc sc t trong t bo thc vt Pht hin thuc tr su, thuc dit
cn trng trong thc n. Nhn bit nhng ha cht trong mt cht cho sn Gim st
cc phn ng hu c Quan st cc vt xut hin, tnh gi tr Rf v tin hnh nh
tnh, pht hin tp cht hoc nh lng. Vic sc k lp mng c tin hnh trong iu
kin chun ho cho kt qu c tin cy cao hn. Hin nay ngi ta thng tin hnh
sc k vi s gip ca h thng sc k lp mng hiu nng cao HPLC.7
ng dng
nh gi Nng, 7/2011
Kim nghim dc phm
Nhm 4
i lng c trng cho mc di chuyn ca cht phn tchl h s di chuyn Rf c
tnh bng t l gia khong dch chuyn ca cht th v khong dch chuyn ca dung
mi
Trong : a: khong cch t im xut pht n tm ca vt mu th, tnh bng cm.
b: khong cch t im xut pht n mc dung mi o trn cng ng i ca vt, tnh
bng cm. Rf: Ch c gi tr t 0 n l.
Nng, 7/2011
8
TNG QUAN
Kim nghim dc phm
Nhm 4
Phng php quang ph hp ph t ngoi da trn kh nnghp ph chn lc cc bc x
chiu vo dung dch ca cht phn tch trong mt dung mi nht nh Tu theo bc
sng, nh sng c chia thnh nhiu vng sng: Vng UV: 200 400 nm Vng VIS:
400 800 nm
Nng, 7/2011
9
TNG QUAN
Kim nghim dc phm
Nhm 4S hp th bc x t ngoi v trng thy: Phn t ca cc cht c kh nng hp
th mt cch chn lc cc bc x chiu qua n. Ph hp th rt phc tp, khng c dng
vch sc nhn m l nhng bng ph tri rng. Trong phn t, cc e c vai tr khc
nhau: tham gia lin kt gi l in t ha tr, khng tham gia lin kt gi l cc
in t c thn. Cc e ha tr c th to lin kt hoc ; cc e khng tham gia lin
kt lp v e ngoi. Khi e ha tr tham gia lin kt s to thnh cc obital lin
kt v obital phn lin kt ( v *, v *); trong obital c nng lng thp nht
cn obital * c mc nng lng cao nht. Trong iu kin thng cc e mc nng lng
thp nht. Khi phn t hp th nng lng, cc e t mc nng lng thp chuyn ln mc
nng lng cao Khi phn t hp th bc x in t gy ra cc bc chuyn nng lng in
t to nn hiu ng ph hp th.
** n
Nng, 7/2011
10
TNG QUAN
Kim nghim dc phm
Nhm 4
nh lut c bn ca s hp th
nh sng (nh lut Lambe-Bia): Chiu mt chm tia n sc c cng I0 qua
dung dch c chiu dy 1. Sau khi b hp th, cng chm tia cn li I. H thc:
lg(Io/I) = A = K.CTrong : k l h s hp th ph thuc vo cu to ca cht tan
trong dung dch. A l mt quang C l nng dung dch Nng, 7/2011 11
TNG QUAN
Kim nghim dc phm
Nhm 4My trc quang UV-Vis:
Ch thch: 1. H tn sc 2. Ngun chiu sng 3. Cuvt ng dung dch (mu) 4.
Detect (t bo quan in, nhn quang) 5. B ghi o (a. in k, b. my t ghi
hay hin s, c. my tnh) Nng, 7/2011
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Kim nghim dc phm
Nhm 4
My sc k lp mng
My quang ph hp ph
Nng, 7/2011
13
Kim nghim dc phm
Nhm 4
Chng 2: Phn thc nghim (Clopheniramin)
nh tnh ( Sc k lp mng)
nh lng (Quang ph hp th t ngoi)
Nng, 7/2011
14
THC NGHIM
Kim nghim dc phm
Nhm 4Phng php sc k lp mng Bn mng: Silica gel GF254, sy 1050C
trong 30 pht trc khi s dng. Dung mi: Axit axetic 1M metanol etyl
axetat (20:30:50) Dung dch th: Lc k mt lng bt vin khong 5mg
clorpheniramin maleat vi cloroform, lc, bay hi dch lc n cn. Ha tan
cn trong 1 ml choroform Dung dch so snh: Dung dch clorpheniramin
maleat chun i chiu 0,5% trong cloroform. Cch tin hnh: Chm ln lt 2 l
mi dung dch trn ln bn mng. Sau khi trin khai, ly bn sc k ra, kh
ngoi khng kh v quan st di nh sng t ngoi bc sng 254 nm. Hai vt chnh
trn sc k ca dung dch th phi tng ng v v tr v mu sc vi hai vt chnh
trn sc k ca dung dch so snh. Sau , phun dung dch kali iodobismuthat
ln bn sc k. Vt chnh thu c trn sc k ca dung dch th phi tng ng v v tr
v mu sc vi vt chnh trn sc k ca dung dch so snh. Nng, 7/2011
Tp cht lin quan Bn mng: Silicagel GF254 Dung mi khai trin:
ietylamin cloroform xiclohexan (10:40:50) Dung dch (1): Lc k mt lng
bt vin tng ng khong 50 mg clorpheniramin maleat vi cloroform, lc,
bay hi dch lc n cn. Ha tan cn trong 1 ml choroform. Dung dch (2):
Pha long 1 th tch dung dch (1) vi cloroform thnh 500 th tch. Cch
tin hnh: Chm ln lt 10 l mi dung dch trn ln bn mng. Trin khai sc k n
khi dung mi i c khong 12 cm. Ly bn sc k ra, kh ngoi khng kh v quan
st di nh sng t ngoi bc sng 254 nm. Nhng vt ph trn sc k ca dung dch
(1) khng c m mu hn vt trn sc k ca dung dch (2) (0,2%). Loi b cc vt
ti im xut pht.
15
THC NGHIM
Kim nghim dc phm
Nhm 4 Cn chnh xc mt lng bt vin khong 3 mg clorpheniramin maleat
vo bnh gn c cha sn 20 ml dung dch axit sulfuric 0,05 M; lc k 5 pht,
thm 20 ml eter. Lc k v lc. Chit lp eter vi 10 ml dung dch axit
sulfuric 0,05 M. Ra phu v lc bng dung dch acid sulfuric 0,05 M. Kim
ha dch lc v dch ra bng dung dch natri hydroxyd 1M n khi lm xanh giy
qu, lc u,chit 2 ln, mi ln vi 50 ml eter, ra dch chit eter vi 20 ml
nc. Ly dch chit ether, chit 3 ln vi dung dch acid sulfuric 0,25 M
theo t l 20: 20: 5. Ly dch chit axit vo bnh nh mc 50 ml, thm dung
dch axit sulfuric 0,25 M ti nh mc, lc u. Ly chnh xc 10 ml dung dch
ny pha long vi dung dch acid sulfuric 0,25 M va 25 ml, lc u v lc. o
hp th ca dung dch thu c bc sng 265 nm, cc o dy 1 cm, dng dung dch
acid sulfuric 0,25 M lm mu trng. Tnh hm lng clorpheniramin maleat,
C16H19ClN2, theo A (1%,1 cm). Ly 212 l gi tr A (1%, 1 cm) bc sng cc
i 265 nm.16
Nng, 7/2011
him im ng m K c ph d
Nng, 7/2011
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Kim nghim dc phm
