Am.  Jour.  Pharm.  ) 
October,  1909.  ]" 
Headache  Mixtures. 
48  L 
method  in  the  hands  of  as  many  chemists  interested  in  this  line  of 
work  as  could  assist.  A  circular  letter  requesting  co-operation  was 
sent  out,  and  a  gratifying  number  responded,  signifying  their  will- 
ingness to  assist,  eleven  of  whom  sent  in  results.  All  who  expressed 
a  desire  to  co-operate  were  supplied  with  a  sample  of  a  mixture 
containing  known  amounts  of  acetanilid,  sodium  bicarbonate,  and 
caffein,  with  the  following  instructions,  the  U.  S.  Pharmacopoeia, 
eighth  revision,  as  amended  and  corrected  May  I  and  June  i,  1907, 
"being  used  as  a  basis  for  all  calculations  and  reagents  unless  other- 
wise specified : 
SEPARATION    OF    CAFFEIN,    ACETANILID,    AND    SODIUM  BICARBONATE. 
Caffein. 
Weigh  out  about  0.3  Gm.  of  headache  powder  on  a  small 
(5.5  cm.)  tared  filter,1  wash  with  successive  small  portions  of  chlo- 
roform to  the  amount  of  about  30  ex.,  collecting  the  solvent  in  a 
100  c.c.  Erlenmeyer.  Distil  off  chloroform  by  means  of  a  small 
flame  until  only  a  few  cubic  centimetres  remain.  Add  10  c.c.  of 
dilute  sulphuric  acid,  then  continue  the  distillation  till  all  the  chloro- 
form has  gone  over,  disconnect  from  condenser,  heat  gently,  first 
on  wire  gauze  to  complete  solution,2  finally  on  a  steam  or  hot-water 
bath  until  the  contents  of  the  flask  have  evaporated  to  about  3  to 
4  c.c.  Cool,  transfer  by  washing  with  water  to  a  separatory  funnel, 
so  that  the  final  volume  does  not  greatly  exceed  20  c.c.  Add  four 
times  the  volume,  or-  about  80  c.c.  of  chloroform,  shake  for  some 
time  vigorously,  allow  to  stand  until  the  chloroform  clears  perfectly, 
pass  through  a  small  dry  filter  into  a  dry  100  c.c.  Erlenmeyer,  distil 
off  the  solvent,  and  use  distillate  for  a  second  extraction,  observing 
the  same  method  of  shaking,  clearing,  and  filtering  as  above  noted. 
Distil  off  chloroform  to  a  small  volume,  transfer  residue  to  a  small 
tared  beaker  or  crystallizing  dish  by  means  of  a  few  cubic  centi- 
metres of  chloroform.    Allow  to  evaporate  spontaneously,  or  if 
1  In  cases  of  powder  mixtures  or  tablets  containing  ground  celery  seed, 
much  coloring  matter,  cinchona  alkaloids,  laxative  or  extractive  principles 
other  than  acetanilid  or  phenacetin,  it  is  our  practice  to  shake  out  the  latter 
by  means  of  chloroform  from  dilute  sulphuric  acid  solution. 
2  In  case  the  preparation  contains  ground  celery  seed  or  certain  oily  prin- 
ciples, it  sometimes  happens  that  the  acid  solution  does  not  become  entirely 
clear  at  this  point. 
