Am.  Jour.  Pharm.  > 
January.  1907.  ) 
Estimation  of  Strychnine  in  Nux  Vomica. 
5 
down  the  side  of  the  beaker.  It  formed  a  distinct  colorless  layer 
at  the  bottom  which  showed  no  trace  of  color  in  several  hours. 
To  another  portion  of  the  brucine  solution  I  c.c.  of  a  solution  of 
sodium  nitrite  was  added.  A  reddish  tint  developed  slowly,  since,  as 
pointed  out  by  Lunge,10  pure  nitrous  acid  does  not  affect  brucine.  A 
few  drops  of  solution  of  hydrogen  peroxide  added  to  the  above 
mixture  produced  a  bright-red  color  immediately  by  partially  oxi- 
dizing the  nitrous  acid  into  nitric  acid  and  other  oxides  of  nitrogen. 
From  these  reactions  we  concluded  that  the  most  suitable  reagent 
for  nitrating  the  brucine  would-  be  nitric  acid  containing  a  fair  pro- 
portion of  the  lower  oxides  of  nitrogen  in  solution. 
We  therefore  modified  the  U.S.P.  process  by  substituting  fuming 
nitric  acid  (commercial  nitrous  acid  S.G.  1-42)  for  the  U.S.P.  nitric 
acid  (S.G.  1*40)  and  extending  the  period  of  contact  to  30  minutes 
in  order  to  insure  destruction  of  the  whole  of  the  brucine  at  various 
temperatures.    The  results  were  as  follows  : — 
Temp.  Time.      Alkaloid  Recovered . 
Brucine,  0*196  gm  .....  6o°  F.  30  min.  none. 
Strychnine,  0*0963   93°  F.        30    "  0*09628 
Mixture  \  Brucine,  0*20  -  .  .  ..  Y      87°  F.        20    «'  0*0941 
I  Strychnine,  0*0942  .  > 
Inasmuch,  however,  as  commercial  nitrous  acid  is  unstable  and  of 
varying  composition,  we  considered  it  desirable  to  discard  its  use  in 
favor  of  U.S.P.  nitric  acid  and  sodium  nitrite.  By  these  reagents 
the  following  results  were  obtained  with  pure  alkaloids: — 
Brucine,  0*203  gm  
Brucine,  0*198  gm  
Strychnine,  0123  gm  
Mixed  |Brucine:°' 134 -m-  •  • 
I  Strychnine,  0*112  gm. 
Mixed{Brncine'OI52^ms-  • 
I  Strychnine,  0*091  gm  . 
These  results  show  that  the  U.S.P.  process  modified  in  this  way 
is  accurate  over  a  wide  range  of  temperature  when  pure  alkaloids 
are  employed.  It  has  been  observed  that  any  impurity  in  the  mix- 
ture of  total  alkaloids  from  nux  vomica  has  a  tendency  to  retard  the 
nitration  of  the  brucine.    Again  if,  as  has  been  suggested,  there  is  a 
Temp. 
Time. 
Alkaloid  Recovered. 
6o°  F. 
20  min. 
None. 
63°  F. 
20  " 
<  < 
900  F. 
30  « 
0*1229 
650  F. 
20  " 
0*1118 
900  F. 
30  " 
0  091 
Ztschr.f.  angew.  Chern.,  1902,  No.  1. 
