462 
Some  Alkaloidal  Assays. 
J  Am.  Jour.  Pharm. 
I     October.  1906. 
immiscible  solvent  a  mixture  of  two  volumes  of  ether  and  one  volume 
of  petroleum  ether  was  used. 
The  results  obtained  from  samples  prepared  in  our  laboratory  from 
drugs  of  good  quality  were  as  follows : 
Fluid  Extract  Aconite  1*20 
"  <f     Coca  076 
"  "     Belladonna  root  o-6o 
"  "     Ipecac  1 -So 
FLUID  EXTRACT  PILOCARPUS. 
Owing  undoubtedly  to  the  solubility  of  pilocarpine  in  water  and 
to  the  tendency  of  this  fluid  extract  to  emulsify,  the  Pharmacopoeia 
directs  to  evaporate  the  fluid  extract  on  sand  and  then  extract  the 
sand  with  chloroform  in  presence  of  ammonia.  A  much  quicker 
method  is  as  follows  :  To  10  c.c.  of  the  fluid  extract  placed  in  sepa- 
rating funnel  No.  I  add  10  c.c.  of  a  saturated  solution  of  potassium 
carbonate  and  shake  out  the  liquid  three  times  with  a  mixture  of 
three  volumes  of  ether  and  one  volume  of  chloroform,  using  40  c.c. 
each  time.  Filter  the  ethereal  liquid  into  separatory  funnel  No.  2, 
concentrate  to  about  one-half,  dilute  with  ether  and  shake  out  with 
standard  acid.  The  excess  of  acid  is  titrated  as  usual.  A  sample 
obtained  from  S.  and  D.  gave  0-53  per  cent. 
FLUID  EXTRACT  CINCHONA. 
Owing  again  to  the  tendency  of  this  fluid  extract  to  emulsify  the 
Pharmacopoeia  directs  to  mix  the  fluid  extract  with  ether,  chloroform 
and  ammonia  and  then  draw  off  an  aliquot  part  for  the  assay.  As 
the  use  of  aliquot  parts  of  ethereal  liquids  is  objectionable,  wherever 
it  can  be  avoided  I  use  the  following  method : 
To  5  c.c.  of  the  fluid  extract  placed  in  funnel  No.  1  add  2  c.c.  of 
a  10  per  cent,  solution  of  sodium  hydroxide  and  shake  out  three 
times  with  a  mixture  of  three  volumes  of  ether  and  one  volume  of 
chloroform,  using  25  c.c.  each  time.  Filter  ethereal  solution  into 
another  separating  funnel  and  shake  it  out  three  times  with  dilute 
sulphuric  acid.  From  the  acid  solution  the  alkaloids  are  extracted 
with  chloroform  in  presence  of  any  alkali,  the  chloroform  distilled 
off  from  a  tared  vessel  and  the  residue  dried  and  weighed.  No 
emulsion  occurs  during  the  process.  A  sample  of  fluid  extract  pre- 
pared in  our  laboratory  gave  4  8 1  per  cent,  total  alkaloids. 
