Am.  Jour.  Pharm. ) 
October,  1906.  J 
Some  Alkaloidal  Assays. 
461 
estimation  by  a  gravimetric  one,  the  acid  liquid  can  be  received  into 
a  separating  funnel  of  suitable  capacity  and  the  titration  carried  out 
directly  in  this  funnel.  After  the  titration  the  liquid  is  made 
strongly  alkaline  with  sodium  hydroxide  and  shaken  out  three 
times  with  chloroform.  The  indicator  added  all  remains  in  the 
alkaline  aqueous  liquid  and  the  colorless  chloroformic  solution,  after 
evaporation,  leaves  the  alkaloid  to  be  weighed  and  identified  by 
special  reactions.  Assayed  by  this  method  a  sample  of  good 
aconite  root  gave  (volumetrically)  1*02  per  cent,  alkaloids. 
IPECAC  ROOT. 
Put  5  grammes  ipecac  (No.  60  powder)  into  shaking  tube,  add 
2-5  c.c.  of  a  10  per  cent,  solution  of  sodium  carbonate  and  25  c.c.  of 
the  same  immiscible  solvent  as  was  used  for  aconite.  After  shaking 
one  hour  percolate  to  exhaustion.  Shake  out  percolate  three  times 
with  small  quantities  of  very  dilute  sulphuric  acid,  add  excess  of 
sodium  hydroxide  and  shake  out  three  times  with  chloroform  ether. 
Distil  the  ethereal  solution  to  about  one-half,  dilute  with  ether  to 
about  original  volume  and  finish  as  with  aconite  root. 
A  good  sample  of  ipecac  assayed  by  this  method  gave  2-55  per 
cent,  alkaloid. 
An  attempt  to  assay  belladonna  leaves  by  this  method  showed 
that  the  leaves  cannot  be  exhausted  if  sodium  carbonate  is  used. 
(Sodium  hydroxide  was  not  tried.) 
FLUID  EXTRACTS. 
These  were  assayed  as  follows : 
From  5  to  20  c.c.  of  the  fluid  extract  were  shaken  out  three  times 
with  the  immiscible  solvents,  using  30,  20  and  20  c.c.  and  making 
the  liquid  alkaline  with  10  per  cent,  solution  of  sodium  carbonate 
in  separating  funnel  No.  1.  The  immiscible  solvent  was  filtered 
into  separatory  funnel  No.  2  and  after  concentration  to  about  one- 
half  and  dilution  with  ether  shaken  out  with  excess  of  standard  acid 
and  then  washed  twice  with  water.  The  excess  of  acid  was  titrated 
in  the  usual  way.  The  whole  volumetric  assay  of  a  fluid  extract  by 
this  method  occupies  about  two  hours.  The  method  works  very 
well  with  the  following  fluid  extracts :  Aconite  root,  belladonna  root, 
coca  leaves  and  ipecac  root.  For  ipecac  5  c.c.  and  for  belladonna 
root  20  c.c.  were  taken;  for  aconite  or  coca  10  c.c.  were  taken.  As 
