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Univ. of Tanta Third Year Pharmacy


Faculty of Pharmacy Pharm. Chem. (II)
Dept. of Pharm. Chem. Practical Sessions
_____________________________________________________________________
ssay of propantheline !romide ta!. (USP "")
O
COOCH
2
CH
2
N(CH(CH
3
)
2
)
2
CH
3
+
. Br
-
(2-Hydroxyethyl)diisopropylmethylammonium bromide xanthene--!arboxylate.
Use# "ntispasmodi!.
Principle# Non-a#ueous a!id $base titration.
ssay#
%ei&h and 'inely po(der )* propantheline bromide tablets. %ei&h a!!urately
a portion o' the po(der e#ui+alent to about ,** m& o' propantheline bromide- and
trans'er to a sintered &lass 'unnel. %ash the po(der (ith ,* ml o' ether. .epeat the
ether (ashin& 'or 'urther t(o times. Combine the ether (ashin&s and use it 'or the test
o' xanthanoi! a!id. /n the same manner extra!t the assay spe!imen (ith 'our ,* ml
portions o' CHCl
3
and e+aporate !are'ully on a (ater bath until only a hea+y oil
remains. Cool and then dissol+e the remainin& oil in a mixture o' 2* ml o' &la!ial
a!eti! a!id and ,0 ml o' mer!uri! a!etate- (armin& sli&htly i' ne!essary to e''e!t
solution. Cool to room temperature and titrate (ith *.,N per!hlori! a!id usin& !rystal
+iolet solution as indi!ator. 1er'orm a blan2 determination and ma2e ne!essary
!orre!tion. 3a!h ml o' *.,N per!hlori! a!id is e#ui+alent to )).*) m& o'
C
23
H
3*
BrNO
3
.
$imit# 1ropantheline bromide tablets !ontain not less than 0.* per!ent and not more
than ,*0.* per!ent o' labeled amount.
2
%esults#
Calculation#
Comment#
3
ssay of &allamine triethiodide ampoules (USP"")
O
O
O
N3t
3
N3t
3
N3t
3
. 3/
-
+
+
+
,-2-3-4ris(-diethylaminoethoxy)ben5ene triehtiodide.
Use# 6us!le relaxant.
Principle# Colorimetry by a!id-dye te!hni#ue.
7O
2
O
OH
Br
Br
HO
Br
Br
H
3
C
CH
3
7O
3
-
C
O
Br
Br
HO
Br
Br
H
3
C
CH
3
N
+
.
)
Complexation
(ith &allamine
Bromo!resol &reen
"!id-dye !omplex (extra!table
(ith !hloro'orm)
ssay#
8ilute an a!!urately measured +olume o' &allamine triethiodide in9e!tion
()*m&:ampoule)- e#ui+alent to about )* m& o' &allamine triethiodide- (ith (ater to
20* ml- and mix. 1ipette 0 ml o' this solution into ,20 ml separator. 4o (hi!h add ,*
ml o' pH 0.3 phosphate bu''er and 0 ml o' a solution o' bromo!resol &reen- extra!t
the !ontent o' the separator (ith 'our 2* ml portions o' !hloro'orm 'ilterin& the
extra!t throu&h a (hattman 'ilter paper into a ,** ml +olumetri! 'las2. 8ilute the
!ombined extra!ts in the +olumetri! 'las2 (ith !hloro'orm to +olume- and mix.
8etermine the absorban!e o' the solution in , !m !ell at the (a+elen&th o' maximum
absorban!e at about ),; nm- (ith a suitable spe!trophotometer usin& !hloro'orm as
the blan2.
$imit# <allamine triethiodide in9e!tion !ontains not less than 0.* per!ent and not
more than ,*0.* per!ent o' labeled amount.
4
%esults#
Calculation#
Comment#
5
ssay of epinephrine (adrenalin) in'ection
NHCH
3
HO
HO
OH
.-(-)-3-)-8ihydroxy--=(methylamino)methyl>ben5yl al!ohol.
Use# /t is the dru& o' !hoi!e in the mana&ement o' aller&i! emer&en!ies- su!h as
anaphylaxis- an&ioneuroti! edema- &iant urti!aria and serum si!2ness.
$imit# 0-,*0?.
Principle# Colorimetry a'ter !helation (ith @e
2+
.
@e
2+
NHCH
3
-
O
-
O
OH
NHCH
3
HO
HO
OH
@erro-!itrate solution
"l2aline bu''er
ssay preparation# 4rans'er to 20 ml +olumetri! 'las2 an a!!urately measured
+olume o' the in9e!tion under assay- e#ui+alent to about , m& o' epinephrine- dilute
(ith sodium bisul'ite (, in 0**) to +olume and mix.
Procedure# /nto t(o 0* ml stoppered !oni!al 'las2s- trans'er- separately- 2*.* ml
ali#uots o' the assay preparation and sodium bisul'ite solution (, in 0**) to pro+ide
the blan2. 4o ea!h 'las2 add *.) ml o' @erro-!itrate solution and ) ml o' Bu''er
solution- mix and allo( the solutions to stand 'or 3* minutes. 8etermine the
absorban!es o' the solutions in 0 !m !ells at the (a+elen&th o' maximum absorban!e
at about 03* nm- (ith a suitable spe!trophotometer- usin& the blan2 to set the
instrument. Cal!ulate the #uantity- in m& o' epinephrine (C

H
,3
NO
3
) in ea!h ml o' the
in9e!tion ta2en by the 'ormula (,A3.2,:333.2) (*.*0*:+)("u:"s). /n (hi!h ,*3.2,
and 333.2 are the mole!ular (ei&hts o' epinephrine bitartrate- respe!ti+ely- C is the
standard preparation- and B is the +olume- in ml- o' /n9e!tion ta2en.
6
%esults#
Calculation#
Comment#
7
ssay of acetylcholine chloride solution
+
N
CH
3
H
3
C
CH
3
O C CH
3
O
. Cl
-
Choline !hloride a!etate.
Use# 1rin!ipally a topi!al ophthamolo&i!al dru& to indu!e miosis and as a resear!h
tool.
Principle#
(,) ( cetyl# .esidual a!id-base titration.
N
CH
3
H
3
C
CH
3
O C CH
3
O
+
xss NaOH
N
CH
3
H
3
C
CH
3
OH
+
+ CH
3
COONa
NaOH + HCl NaCl + H
2
O
(2) ( Chloride# "r&entometry by Bolhard method.
"&
+
+ Cl
-
"&Cl
"&
+
+ 7CN
-
"&7CN
@e
3+
+ 7CN
-
@e(7CN)
;
3-

8
ssay#
( cetyl#
4rans'er ,* ml o' a!etyl!holine !hloride solution into a stoppered !oni!al
'las2. "dd 20.* ml o' *.,N sodium hydroxide- and heat on a steam bath 'or 3*
minutes. /nsert the stopper- allo( to !ool- add phenol phethalein 47- and titrate the
ex!ess al2ali (ith *.,N sul'uri! a!id. 8etermine the exa!t normality o' the *.,N
sodium hydroxide by titratin& 2*.* ml a'ter it has been treated in the same manner as
in the test. 3a!h ml o' *.,N sodium hydroxide is e#ui+alent to ).3*0 m& o' CH
3
CO
bet(een 2*? and 2,? is 'ound.
( Chloride#
4rans'er ,* ml o' a!etyl!holine !hloride solution into a stoppered- ,20 ml
'las2. "dd (ith a&itation 2*.* ml o' *.,N sil+er nitrate- then add 0 ml o' nitri! a!id-
'ilter- (ash (ith ,* ml distilled (ater- to the 'iltrate add 2 ml o' 'erri! ammonium
sul'ate 47- and titrate the ex!ess sil+er nitrate (ith *.,N ammonium thio!yanate.
3a!h ml o' *.,N sil+er nitrate is e#ui+alent to 3.00 m& o' Cl.
$imit test for chloride ()P)#
8issol+e the spe!i'ied amount o' the substan!e in (aterC or prepare a solution
as dire!ted in the text- trans'er to a Nessler tube- add , ml o' nitri! a!id (ex!ept (hen
nitri! a!id is used in the preparation o' the solution)- dilute to 0* ml (ith (ater- add ,
ml o' sil+er nitrate 47. 6ix thorou&hly and set aside 'or 0 minutes- prote!ted 'rom
dire!t-sunli&ht. 4he opales!en!e is !ompared (ith the standard solution.
Standard opalescence for chloride ()P)#
4he standard opales!en!e 'or !hlorides is obtained (hen , ml o' *.*, N
hydro!hlori! a!id and , ml o' nitri! a!id are diluted to 0* ml (ith (ater in a Nessler
tube and then addin& , ml o' sil+er nitrate 47- mixin& thorou&hly and settin& aside 'or
0 minutes- prote!ted 'rom dire!t sunli&ht.

9
%esults#
Calculation#
Comment#
10
ssay of *methyldopa ta!lets (USP"")
COOH
HO
HO
CH
3
H
2
N
D-3-(3-)-dihydroxyphenyl-2-methylalanine.
Use# "ntihypertensi+e.
$imit# 0-,*0?.
Principle# Colorimetry a'ter !helation (ith 'errous.
@e
2+ COOH
HO
HO
CH
3
H
2
N
COOH
-
O
-
O
CH
3
H
2
N
@e
2
+
ssay#
%ei&h and 'inely po(der not less than 2* methyldopa tablets. 4rans'er an
a!!urately (ei&hed portion o' the po(der- e#ui+alent to about ,** m& o' methyldopa-
to a ,** ml +olumetri! 'las2- add 0* ml o' *.,N sul'uri! a!id- a&itate by me!hani!al
means 'or ,0 minutes- add the dilute a!id to +olume- and mix. @ilter the solution
re9e!tin& the 'irst 2* ml o' the 'iltrate. 1ipette 0 ml o' this assay preparation into a ,**
ml +olumetri! 'las2- to a se!ond ,** ml +olumetri! 'las2 add 0 ml o' (ater to pro+ide
the blan2. "dd to ea!h 'las2 0 ml o' 'errous tartrate solution and dilute (ith bu''er
solution to +olume. 8etermine the absorban!e at 02* nm- usin& the blan2 in the
re'eren!e !ell. Cal!ulate the #uantity- in m&- o' C
,*
H
,3
NO
)
in the portion o' the tablets
by the 'ormula ,** C ("u:"s).
11
%esults#
Calculation#
Comment#
12
ssay of phenylephrine eye drops
NHCH
3
HO
OH
(-)-m-Hydroxy--=(methylamino)methyl>ben5yl al!ohol hydro!hloride.
$imit# 0-,*0?.
Use# 8e!on&estant (*.,?) and mydriati! (,*?).
Principle# Bromometry.
NHCH
3
HO
OH
+ 3 Br
2
NHCH
3
HO
OH Br
Br Br
Br
2
+ 2 /
-
2 Br
-

+ /
2
/
2
+ 2 7
2
O3
2- 2/
-
+ 7
)
O
;
2-
ssay#
4rans'er , ml o' phenylephrine eye drops into iodine 'las2- add 0*.* ml o'
*.,N bromine B7- then add 0 ml o' hydro!hlori! a!id- and immediately insert the
stopper- sha2e and allo( to stand 'or ,0 minutes. /ntrodu!e #ui!2ly ,* ml o'
potassium iodide solution (,*?)- allo( to stand 'or 0 min. 7ha2e thorou&hly- remo+e
the stopper- and rinse it and the ne!2 o' the 'las2 (ith a small #uantity o' (ater into
the 'las2- titrate the liberated iodine (ith *.,N sodium thiosul'ate B7- addin& 3 ml o'
star!h 47 as the end point is approa!hed. 1er'orm a blan2 determination.
3a!h ml o' *.,N bromine is e#ui+alent to 3.30 m& o' C
,
H
,3
NO
2
.HCl.
13
%esults#
Calculation#
Comment#
14
ssay of disopyramide phosphate capsules
C
N
CONH
2
((CH
3
)
2
CH)
2
NCH
2
CH
2
. H
3
1O
)
-=2-(8iisopropylamino)ethyl>--phenyl-2-pyridinea!etamide phosphate.
Use# "ntiarrhythmi!.
$imit# 0-,*0?.
Principle# EB spe!trophotometry at 2; nm.
ssay#
%ei&h the !ontents o' not less than 2* 8isopyramide phosphate !apsules- and
!al!ulate the a+era&e (ei&ht per !apsule. 6ix the !ombined !ontents o' the !apsules-
and trans'er an a!!urately (ei&hed portion- e#ui+alent to about ,** m& o'
disopyramide phosphate- to a &lass stoppered- ,20 ml 'las2. "dd 20 ml o' 6ethanoli!
sul'uri! a!id- and stir 'or 3* minutes. @ilter throu&h a medium porosity- sintered &lass
'ilter- and rinse thorou&hly (ith methanoli! sul'uri! a!id. 4rans'er the !ombined
'iltrate and (ashin&s to a 0* ml +olumetri! 'las2- dilute (ith methanoli! sul'uri! a!id
to +olume- and mix. 8etermine the absorban!e in , !m !ell at the (a+elen&th o'
maximum absorban!e at about 2; nm (ith a suitable spe!trophotometer- usin&
methanoli! sul'uri! a!id as the blan2.
15
%esults#
Calculation#
Comment#
16
ssay of propranolol hydrochloride ta!lets (USP""I)
O NHCH(CH
3
)
2
OH
. HCl
,-=(,-6ethylethyl)amino>-3-(,-naphthyloxy)-2-propanol HCl.
Use# "ntihypertensi+e- antian&inal and antiarrhythmi!.
$imit# 0-,*0?.
Principle# EB spe!trophotometry at 23 nm.
ssay#
Standard preparation# 8issol+e an a!!urately (ei&hed #uantity o' E71 propranolol
hydro!hloride .7 in (ater- and dilute #uantitati+ely and step(ise (ith (ater to obtain
a solution ha+in& a 2no(n !on!entration o' about 2** m!& per ml.
ssay preparation# %ei&h and 'inely po(der not less than 2* propranolol
hydro!hloride tablets. %ei&h a!!urately a portion o' the po(der- e#ui+alent to about
,** m& o' propranolol hydro!hloride and trans'er (ith the aid o' about 30* ml o'
*.,N hydro!hlori! a!id to a 0** ml +olumetri! 'las2. 7(irl by me!hani!al means 'or
3* minutes- dilute (ith *.,N hydro!hlori! a!id to +olume- mix and !entri'u&e a
portion o' the solution. 4rans'er 0.* ml ea!h o' the 7tandard preparation and the "ssay
preparation to separators- and treat ea!h as 'ollo(sF "dd ,* ml o' (ater- , ml o'
sodium hydroxide solution (, in 0)- and 20 ml o' n-heptane. 7ha2e by me!hani!al
means 'or 0 minutes- and allo( the layers to separate. Con!omitantly determine the
absorban!es o' both n-heptane solutions in , !m !ells at the (a+elen&th o' maximum
absorban!e at about 23 nm- (ith a suitable spe!trophotometer.
17
%esults#
Calculation#
Comment#
18
ssay of ephedrine hydrochloride ta!lets (USP"")
NHCH
3
CH
3
OH
(-)--=,-(methylamino)ethyl>-ben5enemethanol.
Use# Bron!hodilator.
$imit# A-,**.0?.
Principle# Non-a#ueous a!id base titration.
ssay#
@inely po(der 0 ephedrine hydro!hloride tablets (!ontain 3** m&)- dissol+e in
2* ml o' &la!ial a!eti! a!id- and 'ilter. "dd 0 ml o' mer!uri! a!etate to the 'iltrate- and
3 drops o' !rystal +iolet and titrate (ith *.,N per!hlori! a!id to blue end point.
1er'orm a blan2 determination. 3a!h ml o' *.,N per!hlori! a!id is e#ui+alent
to 2*.,G m& o' C
,*
H
,0
NOHCl
19
%esults#
Calculation#
Comment#
20
ssay of phenindione ta!lets (+P ,-..)
O
O
C
;
H
0
2-1henyl-,-3-indandione.
Use# "nti!oa&ulant.
$imit# 0-,*0?.
Principle# EB spe!trophotometry at 2GA nm.
O
O
C
;
H
0
NaOH
O
C
;
H
0
ONa
ssay#
%ei&h and po(der 2* tablets. 7ha2e a #uantity o' the po(der !ontainin& 0*
m& o' phenindione (ith ,0* ml o' *.,N sodium hydroxide 'or , hour and add
su''i!ient *.,N sodium hydroxide to produ!e 20* ml. @ilter and dilute 0 ml o' the
'iltrate to 20* ml (ith *.,N sodium hydroxide. 6easure the absorban!e o' the
resultin& solution at the maximum at 2GA nm. Cal!ulate the !ontent C
,0
H
,*
O
2
ta2in&
,3,* as the +alue o' " (,?- , !m) at the maximum at 2GA nm.
21
%esults#
Calculation#
Comment#
22
$imit of pero/ide in anesthetic ether (+P ,--0)
4rans'er A ml o' potassium iodide and star!h solution to a stoppered tube o'
about ,2 ml !apa!ity and ,.0 !m in diameter. @ill !ompletely (ith the substan!e bein&
examined- sha2e +i&orously- and allo( to stand in the dar2 'or thirty minutes. No
!olor is produ!ed.
Principle# 1eroxide (i' present) oxidi5es iodide to iodine- (hi!h (ill &i+e +iolet !olor
(ith star!h.
%esults#
Comment#
23
ssay of chloroproma1ine hydrochloride ta!lets (+P ,-..)
N
7
Cl
CH
2
CH
2
CH
2
N(CH
3
)
2
. HCl
2-Chloro-,*-=3-(dimethylamino)propyl>phenothia5ine HCl.
Use# "ntipsy!hoti!- antiemeti!.
$imit# 0-,*0?.
Principle# EB spe!trophotometry at 20) nm.
ssay#
Carry out the 'ollo(in& pro!edure prote!ted 'rom li&ht. 1o(der ,* tablets
(ithout loss- triturate the po(der (ith ,* ml o' absolute ethanol- add su''i!ient *.,N
hydro!hlori! a!id to produ!e 20* ml and 'ilter. 8ilute a +olume o' the 'iltrate
!ontainin& 0 m& o' !hloroproma5ine hydro!hloride to ,** ml (ith the same sol+ent.
6easure the absorban!e o' the resultin& solution at the maximum at 20) nm.
Cal!ulate the !ontent o' C
,G
H
,
CDN
2
7- HCl ta2in& ,0 as the +alue o' " (,?- , !m) at
the maximum at 20) nm.
24
%esults#
Calculation#
Comment#
25
ssay of chloral hydrate syrup (USP ""II)
CCl
2
C3(43)
5
Use# 7edati+e-hypnoti!.
$imit# 0-,*0?.
Principle# .esidual a!id $ base titration.
CCl
l3
CH(OH)
2
+ NaOH CHCl
3
+ HCOONa
2 NaOH + H
2
7O
)
Na
2
7O
)
+ 2 H
2
O
ssay#
4rans'er ,0 ml o' !hloral hydrate syrup to a 20* ml !oni!al 'las2 (ith the aid
o' se+eral portions o' (ater. "dd 3* ml o' ,N sodium hydroxide and mix. "'ter the
mixture has stood 'or 2 minutes- add 0 drops o' phenolphthalein 47. "nd immediately
titrate the ex!ess sodium hydroxide (ith ,N sul'uri! a!id. 8esi&nate the +olume o'
,N sodium hydroxide !onsumed as ". 4rans'er ,0 ml o' syrup to a se!ond 20* ml
!oni!al 'las2 (ith the aid o' se+eral portions o' (ater. "dd ,* drops o'
phenolphthalein 47- and titrate (ith *.,N sodium hydroxide. 8esi&nate the +olume o'
*.,N sodium hydroxide B7 !onsumed as B. Cal!ulate the (ei&ht- in m& o' C
2
H
3
Cl
3
O
2
in the amount o' syrup ta2en by the 'irst titration by the 'ormula ,;0.) (" - *.0 B).
26
%esults#
Calculation#
Comment#
27
$imit test for lead
Test # 4o ,2 ml o' the pres!ribed a#ueous solution add 2 ml o' a!etate bu''er pH 3.0
mix- add ,.2 ml o' thioa!etamide rea&ent- mix immediately and allo( to stand 'or 2
minutes. "ny bro(n !olor produ!ed is not more than a mixture o' ,* ml o' either lead
standard solution (, ppm) or lead standard solution (2 ppm)- as pres!ribed- and 2 ml
o' the solution bein& examined. 4he standard solution exhibits a sli&htly bro(n !olor
(hen !ompared to a solution prepared by treatin& in the same manner a mixture o' ,*
ml o' (ater and 2 ml o' the solution bein& examined.
Principle# Dead &i+es bro(n !olor o' 1b7 (hen rea!ts (ith thioa!etamide.
%esults#
Comment#
28
ssay of theophylline ta!lets (+P ,-..)
N
N
N
N
CH
3
H
3
C
O
O
H
3-G 8ihydro-,-3-dimethyl- ,H-purine-2-; dione.
Use# Bron!hodilator.
Principle# EB spe!trophotometry at 2G0 nm.
ssay#
%ei&h and po(der 2* tablets. 7ha2e a #uantity o' the po(der !ontainin& ,**
m& o' theophylline (ith a mixture o' 2* ml o' *.,N sodium hydroxide and ;* ml o'
(ater 'or ,* minutes- add su''i!ient (ater to produ!e 2** ml- mix and 'ilter. 8ilute 0
ml o' the 'iltrate to 20* ml (ith *.*,N sodium hydroxide and measure the absorban!e
o' the resultin& solution at the maximum at 2G0 nm. Cal!ulate the !ontent o'
theophylline ta2in& ;0* as the +alue o' " (,?- , !m) at the maximum at 2G0 nm.
29
%esults#
Calculation#
Comment#
30
ssay of allopurinol ta!lets (+P ,-..)
HN
N N
N
O
H
,-0-8ihydro-)H-pyra5olo=3-)-d>pyrimidin-)-one.
$imit# 0-,*0?.
Use# " stru!tural analo& o' hypoxanthine used in the treatment o' &out. /t inhibits uri!
a!id 'ormation +ia inhibition o' xanthine oxidase en5yme.
Principle# EB spe!trophotometry at 20* nm.
HN
N N
N
O
H
N
N N
N
H
OH
NaOH
ssay#
%ei&h and po(der 2* tablets. 7ha2e a #uantity o' the po(der !ontainin& *., &
o' allopurinol (ith 2* ml o' *.*0N sodium hydroxide 'or 2* minutes- add A* ml o'
*.,N hydro!hlori! a!id- sha2e 'or ,* minutes- add su''i!ient *.,6 hydro!hlori! a!id
to pro!edure 20* ml- and 'ilter. 8ilute ,* ml o' the 'iltrate to 20* ml (ith *.,N
hydro!hlori! a!id. 6easure the absorban!e o' the resultin& solution at the maximum
at 20* nm- usin& *.,N hydro!hlori! a!id in the re'eren!e !ell. Cal!ulate the !ontent o'
C
0
H
)
N
)
O ta2in& 0;3 as the +alue o' " (,?- , !m) at the maximum at 20* nm.
31
%esults#
Calculation#
Comment#
32
ssay of i!uprofen ta!lets (+P ,-..)
COOH
CH
3
H
3
C
CH
3
(H)-2-(p-isobutylphenyl)propioni! a!id.
Use# N7"/8.
$imit# 0-,*0?
Principle# 8ire!t a!id-base titration.
ssay#
%ei&h and po(der 2* tablets. 3xtra!t a #uantity o' the po(der !ontainin& *.2
& o' ibupro'en (ith ,* ml !hloro'orm 'or ,0 minutes and 'ilter throu&h a 'ilter paper.
%ash the residue (ith ,* ml o' !hloro'orm and &ently e+aporate the !ombined
'iltrates 9ust to dryness in a !urrent o' air. 8issol+e the residue in 3* ml o' ethanol
(;?) pre+iously neutrali5ed to phenolphthalein solution and titrate (ith *.,N sodium
hydroxide usin& phenolphthalein solution as indi!ator. 3a!h ml o' *.,N sodium
hydroxide is e#ui+alent to *.*2*;3 & o' C
,3
H
,A
O
2
33
%esults#
Calculation#
Comment#
34
ssay of paracetamol (acetaminophen) ta!lets (+P ,-..)
NHCOCH
3
OH
N-"!etyl-p-aminophenol.
Use# "nal&esi!-antipyreti! a&ent.
$imit# 0-,*0?.
Principle# EB spe!trophotometry at 20G nm.
ssay#
%ei&h and po(der 2* tablets. "dd a #uantity o' the po(der !ontainin& *.0 &
o' para!etamol to 0* ml o' *.,N sodium hydroxide- dilute (ith ,** ml o' (ater- sha2e
'or ,0 minutes and add su''i!ient (ater to produ!e 20* ml. 6ix- 'ilter and dilute 0 ml
to ,** ml (ith (ater then dilute 2 ml to ,** ml (ith (ater and measure the
absorban!e o' the resultin& solution at the maximum at 20G nm. Cal!ulate the !ontent
o' C
A
H

NO
2
ta2in& G,0 as the +alue o' " (,?- , !m) at the maximum at 20G nm.
35
%esults#
Calculation#
Comment#
36
$imit of salicylic acid in aspirin ta!lets
7ha2e a #uantity o' the po(dered tablets !ontainin& 3** m& o' aspirin (ith )
ml o' ethanol (;?) and dilute to ,** ml (ith (ater at a temperature not ex!eedin&
,*
o
C. @ilter immediately- trans'er 0* ml o' the 'iltrate to a Nessler !ylinder- add , ml
o' 'reshly prepared a!id ammonium iron (///) sul'ate solution- mix and allo( to stand
'or , minute. "ny +iolet !olor produ!ed is not more intense than that produ!ed by
addin& , ml o' 'reshly prepared a!id ammonium iron (///) sul'ate solution to a mixture
o' ).0 ml o' a 'reshly prepared *.*,? solution o' sali!yli! a!id- 2 ml o' ethanol (;?)
and su''i!ient (ater to produ!e 0* ml !ontained in a se!ond Nessler !ylinder (*.3?).
Principle# "ny sali!yli! a!id present in aspirin (ill produ!e +iolet !olor (ith @e
3+
.
%esult#
Comment#
37
ssay of aspirin ta!lets (+P ,-..)

COOH
OCOCH
3
"!etylsali!yli! a!id.
Use# N7"/8.
$imit# 0-,*0?.
Principle# .esidual a!id-base 4itration.
COOH
OCOCH
3
NaOH
COONa
ONa
NaOH + HCl NaCl + H
2
O
ssay#
%ei&h and po(der 2* tablets. 4o a #uantity o' the po(der !ontainin& 3** m&
o' aspirin add 3* ml o' *.0N sodium hydroxide- boil &ently 'or ,* minutes and titrate
the ex!ess o' al2ali (ith *.0N hydro!hlori! a!id usin& phenol red solution as
indi!ator. .epeat the operation (ithout the substan!e bein& examined. 4he di''eren!e
bet(een the t(o experiments represents the amount o' sodium hydroxide re#uired .
3a!h ml o' *.0N sodium hydroxide is e#ui+alent to *.*)0*) & o' C

H
A
O
)
38
%esults#
Calculation#
Comment#
39
ssay of mefenamic acid capsules
NH
COOH
CH
3
CH
3
2-=(2-3-8imethylphenyl)amino>ben5oi! a!id.
Use# N7"/8.
$imit# 2.0-,*G.0?
Principle# "!id-base titration.
ssay#
8issol+e the !ontent o' one !apsule (20* m&) in ,** ml o' absolute ethanol
pre+iously neutrali5ed to phenolphthalein solution and titrate (ith *.,N sodium
hydroxide usin& phenol red solution as indi!ator. 3a!h ml o' *.,N sodium hydroxide
is e#ui+alent to *.*2),3 & o' C
,0
H
,0
NO
2
.
40
%esults#
Calculation#
Comment#
41
ssay of furosemide in'ection (USP""II)
COOH
Cl
H
2
N7
O
O
NHCH
2
O
)-Chloro-N-'ur'uryl-0-sul'amoylanthranili! a!id.
Use# Doop diureti!.
Principle# EB spe!trophotometry at 2G, nm.
ssay#
I @urosemide in9e!tion is a sterile solution o' 'urosemide in (ater o' in9e!tion
prepared (ith the aid o' sodium hydroxide. /t !ontains not less than 0.* per!ent and
not more than ,*0.* per!ent o' the labeled amount o' C
,2
H
,,
CiN
2
O
0
7
4rans'er to a ,** ml +olumetri! 'las2 an a!!urately measured +olume o'
'urosemide /n9e!tion- e#ui+alent to about )* m& o' 'urosemide- dilute (ith (ater to
+olume- and mix. 8ilute 2 ml o' this solution (ith *.*2N sodium hydroxide in a
se!ond ,** ml +olumetri! 'las2 to +olume- and mix. 8issol+e about ,* m& o' E71
'urosemide .7- a!!urately (ei&hed- in ; ml o' *.,N sodium hydroxide in a 20 ml
+olumetri! 'las2- and dilute (ith (ater to +olume. 8ilute 2 ml o' the resultin& solution
#uantitati+ely (ith *.*2N sodium hydroxide to obtain a standard solution ha+in& a
2no(n !on!entration o' about A m!& per ml. Con!omitantly determine the
absorban!es o' both solutions in , !m !ells at the (a+elen&th o' maximum
absorban!e at about 2G, nm- (ith a suitable spe!trophotometer- usin& *.*2N sodium
hydroxide as the blan2. Cal!ulate the #uantity- in m& o' C
,2
H
,,
ClN
2
O
0
7 in the +olume
o' in9e!tion ta2en by the 'ormula 0C ("u:"s)- in (hi!h C is the !on!entration- in m!&
per ml- o' E71 'urosemide .7 in the standard solution- and "u and "s are the
absorban!es o' the solution 'rom 'urosemide in9e!tion and the standard solution-
respe!ti+ely.
42
%esults#
Calculation#
Comment#
43
ssay of ferrous fumarate capsules

CH
HC
C
O
C O
O
-
O
-
@e
2+
Use# 7our!e o' iron in iron de'i!ien!y anemia.
$imit# 0-,*0 ?
Principle# .edox-titration.
ssay#
8issol+e about 2** m& o' 'errous 'umarate !apsules a!!urately (ei&hed in 2*
ml o' dilute sul'uri! a!id and titrate (ith ,N potassium perman&anate till a permanent
pin2 !olor (perman&anate is a sel' indi!ator). 3a!h ml o' ,N potassium perman&anate
is e#ui+alent to *.*,; & o' C
)
H
2
@eO
)
%esults#
Calculation#
44
Comment#
ssay of ascor!ic acid (vitamin C) ta!lets (+P ,-65)
O
OH HO
O
H
CH HO
CH
2
HO

Use# %ater-soluble +itamin.
$imit# 0-,*0?.
Principle# .edox-titration (ith Ce
)+
.
45
O
OH HO
O
H
CH HO
CH
2
HO
+ 2 Ce
)+
+ 2 Ce
3+
O
O O
O
H
CH HO
CH
2
HO
"s!orbi! a!id 8ehydroas!orbi! a!id
ssay#
%ei&h and po(der , tablet. 8issol+e a #uantity o' the po(der e#ui+alent to
*., & o' as!orbi! a!id as !ompletely possible in a mixture o' 3* ml o' (ater and 2* ml
dilute sul'uri! a!id and titrate (ith *.,N ammonium !erium (/B) sul'ate usin& 'erroin
sul'ate solution as indi!ator. 3a!h ml o' *.,N ammonium !erium (/B) sul'ate is
e#ui+alent to *.**AA*; & o' C
;
H
A
O
;
%esults#
Calculation#
46
Comment#
ssay of pilocarpine nitrate ophthalmic solution (USP"")7 (8F "9)
O
O
3t
CH
2
N
N
CH
3
. HCl
3-3thyldihydro-)-=(,-methyl-,H-imida5ol-0-yl)-methyl>-2(3H)-@uranone.
Use# 4reatment o' &lau!oma.
$imit# 0-,*0?.
Principle# Colorimetry by !helation (ith @e
3+
a'ter rea!tion (ith NH
2
OH in al2aline
medium.
O
O
3t
CH
2
N
N
CH
3
NH
2
OH
NaOH
O
3t
.
-
O N
H
OH
3t
.
-
O N
-
O
O
-
@e
3+
ssay#
Standard preparation# 8issol+e about )* m& o' E71 pilo!arpine nitrate .7-
a!!urately (ei&hed- in (ater and add (ater to ma2e ,** ml and mix.
47
ssay preparationF 4rans'er to a separator an a!!urately measured +olume o'
pilo!arpine nitrate ophthalmi! solution e#ui+alent to about )* m& o' pilo!arpine
hydro!hloride- add ,* ml o' (ater- and ad9ust (ith 3N hydro!hlori! a!id to a pH ) i'
ne!essary. 3xtra!t the solution (ith )* ml o' methylene !hloride- and 'ilter the
a#ueous phase into a ,** ml +olumetri! 'las2. %ash the methylene !hloride (ith 0 ml
o' (ater- addin& the (ashin& to the !ontents o' the 'las2- add (ater to +olume and
mix.
Procedure#
4o 0 ml ea!h o' the standard preparation- the assay preparation- and (ater to
pro+ide a blan2- add su!!essi+ely and (ith mixin& a'ter ea!h addition , ml o'
hydroxylamine hydro!hloride solution (G in ,**) and , ml o' sodium hydroxide
solution (G in 0*). "llo( to stand 'or ,* minutes- and to ea!h solution add , ml o' )N
hydro!hlori! a!id and , ml o' a , in 2* solution o' 'erri! !hloride in *.,N
hydro!hlori! a!id. /mmediately add (ater to ma2e ,* ml- and mix. 8etermine the
absorban!es o' the solutions 'rom the assay preparation and the standard preparation
a'ter ,* minutes- a!!urately timed- a&ainst the blan2 in , !m !ells at the (a+elen&th
o' maximum absorban!e at about 0** nm- (ith a suitable spe!trophotometer.
Cal!ulate the #uantity- in m&- o' C
,,
H
,;
N
2
O
2
. HCl in ea!h ml o' the ophthalmi!
solution ta2en by the 'ormula *.**2 (C/V) (Au/As)- in (hi!h C is the !on!entration-
in m!& per ml- o' E71 pilo!arpine nitrate .7 in the standard preparation- V is the
+olume- in ml- o' ophthalmi! solution ta2en- and Au and As are the absorban!es o' the
solutions 'rom the assay preparation and the standard preparation- respe!ti+ely.
48
49
%esults#
Calculation#
Comment#
50
Univ. of Tanta Third Year Pharmacy
Faculty of Pharmacy Pharm. Chem. (II)
Dept. of Pharm. Chem. Practical Sessions
ttendance Sheet
Date )/periment Status :ar; Si&nature