Mr

300.8
A. [2-[(2^S)-4-methyl-2-phenylpiperazin-1-
yl]phenyl]metha- nol.
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E!"#EA$ #%A!MA&"#"E'A (.0 Mianserinhydrochloride
01)200(*084+
M'A$SE!'$ %,-!"&%."!'-E
Mian/erini hy0ro1hlori02m
&
18
%
21
&l$
2
-E3'$'4'"$
Mian/erin hy0ro1hlori0e 1ontain/ not
le// than 58.( per 1ent an0 not more
than the e62i7alent o8 101.0 per 1ent o8
(!S)-2-methyl-1929394910914:-
he;ahy0ro0i:enzo[19)]pyrazino[192a]az
epine hy0ro1hlori0e9 1al12late0 <ith
re8eren1e to the 0rie0 /2:/tan1e.
&%A!A&4E!S
=hite or almo/t <hite9 1ry/talline po<0er or
1ry/tal/9 /parin>ly /ol2:le in <ater9 /ol2:le in
methylene 1hlori0e9 /li>htly /ol2:le in al1ohol.
'-E$4'3'&A4'"$
3ir/t i0enti8i1ation* ?9 -.
Se1on0 i0enti8i1ation* A9 &9 -.
A. -i//ol7e (0.0 m> in water R an0 0il2te to
(0.0 ml <ith the /ame /ol7ent. -il2te (.0 ml
o8 the /ol2tion to (0.0 ml <ith water R.
E;amine0 :et<een 230 nm an0 3(0 nm
(2.2.25), the /ol2tion /ho</ an a:/orption
ma;im2m at 2@5 nm. 4he /pe1i8i1 a:/orption
at the ma;im2m i/ +4 to @2.
?. E;amine :y in8rare0 a:/orption
/pe1trophotometry (2.2.24), 1omparin> <ith
the /pe1tr2m o:taine0 <ith mianserin
hydrochloride CRS. E;amine the /2:/tan1e/ a/
0i/1/ prepare0 2/in> potassium chloride R. '8 the
/pe1tra o:taine0 /ho< 0i88eren1e/9 0i//ol7e
the /2:/tan1e to :e e;amine0 an0 the
re8eren1e /2:/tan1e /eparately in methanol R,
e7aporate to 0ryne// an0 re1or0 ne< /pe1tra
2/in> the re/i02e/.
&. E;amine :y thin-layer 1hromato>raphy
(2.2.27), 2/in> silica gel G
254
R a/ the 1oatin>
/2:/tan1e.
!est solution. -i//ol7e 10 m> o8 the
/2:/tan1e to :e e;amine0 in methylene
chloride R an0 0il2te to ( ml <ith the /ame
/ol7ent.
!e8eren1e /ol2tion (a). "issol#e $% mg o&
mianserin hydrochloride CRS in methylene
chloride R and dilute to 5 ml with the same
sol#ent.
!e8eren1e /ol2tion (:). "issol#e $% mg o&
mianserin hydrochloride CRS and $% mg o&
cyproheptadine hydrochloride CRS in methylene
chloride R and dilute to 5 ml with the same
sol#ent.
Apply to the plate 2 pl o8 ea1h /ol2tion.
-e7elop o7er a path o8 1( 1m 2/in> a mi;t2re
o8 ( 7ol2me/ o8 diethylamine R, 20 7ol2me/ o8
ether R an0 @( 7ol2me/ o8 cyclohe'ane R.
E;amine in 2ltra7iolet li>ht at 2(4 nm. 4he
prin1ipal /pot in the 1hromato>ram o:taine0
<ith the te/t /ol2tion i/ /imilar in po/ition an0
/ize to the prin1ipal /pot in the 1hromato>ram
o:taine0 <ith re8eren1e /ol2tion (a). 4he te/t
i/ not 7ali0 2nle// the 1hromato>ram o:taine0
<ith re8eren1e /ol2tion (:) /ho</ t<o 1learly
/eparate0 prin1ipal /pot/.
-.'t >i7e/ rea1tion (a) o8 1hlori0e/ (2.(.$).
4ES4S
pH (2.2.3). -i//ol7e 0.10 > in car)on dio'ide*
&ree water R an0 0il2te to 10 ml <ith the /ame
/ol7ent. 4he p% o8 the /ol2tion i/ 4.0 to (.(.
Related substances. E;amine :y thin-layer
1hromato>raphy (2.2.27), 2/in> silica gel G R a/
the 1oatin> /2:/tan1e.
!est solution. -i//ol7e 0.20 > o8 the /2:/tan1e to
:e e;amine0 in a mi;t2re o8 1 7ol2me o8
ammonia R an0 4 7ol2me/ o8 methanol R an0
0il2te to 10 ml <ith the /ame mi;t2re o8
/ol7ent/.
Re&erence solution (a). -il2te 1 ml o8 the te/t
/ol2tion to 200 ml <ith a mi;t2re o8 1 7ol2me
o8 ammonia R an0 4 7ol2me/ o8 methanol R.
Re&erence solution ()). -il2te ( ml o8 re8eren1e
/ol2tion (a) to 2( ml <ith a mi;t2re o8 1 7ol2me
o8 ammonia R an0 4 7ol2me/ o8 methanol R.
Apply to the plate ( pl o8 ea1h /ol2tion.
-e7elop o7er a path o8 1( 1m 2/in> a mi;t2re
o8 10 7ol2me/ o8 methanol R an0 50 7ol2me/ o8
methylene chloride R. -ry the plate in a 12rrent o8
1ol0 air. E;po/e the plate to io0ine 7apo2r 8or
20 min. Any /pot in the 1hromato>ram o:taine0
<ith the te/t /ol2tion9 apart 8rom the prin1ipal
/pot9 i/ not more inten/e than the /pot in the
1hromato>ram o:taine0 <ith re8eren1e /ol2tion
(a) (0.( per 1ent) an0 at mo/t one /21h /pot i/
more inten/e than the /pot in the 1hromato>ram
o:taine0 <ith re8eren1e /ol2tion (:) (0.1 per
1ent).
Loss on drying (2.2.32). $ot more than 0.( per
1ent9 0etermine0 on 1.000 > :y 0ryin> o7er
diphosphorus pento'ide R at +( A& at a pre//2re
not e;1ee0in> @00 #a 8or 3 h.
Sulphated ash (2.4.$4). $ot more than 0.1 per
1ent9 0etermine0 on 1.0 >.
ASSA,
-i//ol7e 0.200 > in a mi;t2re o8 (.0 ml o8 %.%$
+hydrochloric acid an0 (0 ml o8 alcohol R. &arry
o2t a potentiometri1 titration (2.2.20)9 2/in> %.$
+ sodium hydro'ide. !ea0 the 7ol2me a00e0
:et<een the t<o point/ o8 in8le;ion.
l ml o8 %.$ + sodium hydro'ide i/ e62i7alent to
30.08 m> o8
&
18
%
21
&l$
2B
S4"!ACE
Store prote1te0 8rom li>ht.
'M#!'4'ES
204
1
Ceneral $oti1e/ (1) apply to all mono>raph/ an0 other
te;t/