Am.  Jour.  Pharnj.  \ 
July.  1907.  J 
Alkaloidal  Assay. 
307 
alcohol  in  which  1-5  grammes  of  tartaric  acid  have  been  previously 
dissolved  ;  add  sufficient  absolute  alcohol  to  make  100  c.c.  Shake 
well,  then  set  aside  for  a  few  minutes.  Filter  ;  transfer  50  c.c.  of  the 
filtrate  to  a  shallow  porcelain  basin  of  a  diameter  of  6  inches  (15  centi- 
meters) and  evaporate  carefully  on  a  water  bath,  rotating  the  contents 
of  the  basin  occasionally,  and  especially  towards  the  end  of  the 
evaporation,  so  that  the  resulting  extract  may  cover  a  large  portion 
of  the  basin.  When  dry,  cool  the  extract  by  floating  the  basin  in 
cold  water  ;  add  10  c.c.  of  half-normal  sulphuric  acid  and  rotate  the 
liquid  about  in  the  dish  until  the  extract  is  dissolved  or  disinte- 
grated ;  set  aside  for  two  minutes.  Filter  the  liquid  through  a 
small,  firmly  packed  pledget  of  cotton-wool  previously  moistened 
with  water,  into  a  large  pear-shaped  separator.  Rinse  the  evapo- 
rating dish  with  two  successive  5  c.c.  portions  of  water,  stirring 
to  disintegrate  the  insoluble  substances,  and  pass  the  liquid  through 
the  filter.  To  the  separator  add  20  c.c.  of  a  mixture  of  16  c.c.  ot 
chloroform  and  4  c.c.  of  ether  ;  add  4  c.c.  or  q.  s.  of  20  per  cent,  solu- 
tion of  KOH,  insert  the  stopper  and  shake  vigorously.  When  the 
fluids  have  separated  draw  off  the  lower  layer  into  a  second  separator 
containing  15  c.c.  of  distilled  water  and,  after  agitation  and  separa- 
tion as  before,  transfer  the  lower  layer  to  a  third  separator  also  con. 
taining  15  c.c.  of  distilled  water;  agitate  and  allow  to  separate. 
Pass  the  lower  layer  through  a  chloroform-moistened  pledget  of 
cotton  wool  into  a  fourth  separator  of  about  150  c.c.  capacity.  In 
the  presence  of  a  volatile  alkaloid  wash  the  cotton  afterwards  with 
5  c.c.  of  chloroform  ;  in  all  cases  the  stems  of  the  separators  should 
be  washed  with  1  c.c.  of  chloroform  after  the  solvent  has  been  run 
off  and  the  washings  added.  Repeat  the  extraction  till  no  more 
alkaloid  is  obtained  with  two  or  more  portions  of  the  immiscible 
solvent,  which  finally  collect,  after  washing  as  before,  in  separator 
N  N 
number  4.    To  the  bulked  ethereal  extract  add  excess  of —  or   
-  50  100 
sulphuric  acid  and  shake  thoroughly.    After  complete  separation 
reject  the  lower  layer ;  add  cochineal  T.  S.  or  solution  of  iodeosin 
•  N 
in  water-saturated  ether  and  titrate  back  with  —  sodium  hydroxide 
50  y 
solution. 
For  solid  extracts. — Dissolve  2  grammes  of  the  extract  in  10  c.c. 
50  per  cent,  alcohol  and  treat  as  a  fluid  extract. 
91  Fulton  Street,  New  York. 
