Am.  Jour.  Pharm. 
June,  1899. 
Hydrastine  Hexiodide. 
263 
of  ammonia  has  disappeared,  and  then  in  a  vacuum  over  sulphuric 
acid  for  about  five  or  six  hours.  The  powder  is  then  put  into  a 
filter  paper  cell,  placed  in  a  Soxhlet  extraction  apparatus,  the  jar 
rinsed  out  several  times  with  powdered  glass,  or,  in  the  absence  of 
this,  with  coarsely  powdered  barium  nitrate,  the  rinsings  added  to 
the  Soxhlet,  the  latter  connected  with  an  Erlenmeyer  flask  contain- 
ing about  40  or  50  c.c.  absolute  ether,  and  the  extraction  conducted 
in  the  usual  way,  till  a  few  drops  after  evaporation  of  the  ether  and 
acidulation  give  no  reaction  with  Mayer's  or  Wagner's  reagent, 
The  ethereal  extract  will  be  found  to  have  only  a  very  slight  yellow 
color.  The  Erlenmeyer  is  then  detached  from  the  Soxhlet,  the  ether 
poured  out  into  a  flat  evaporating  dish,  the  Erlenmeyer  washed  out 
several  times  with  water  containing  about  2  per  cent,  sulphuric  acid, 
the  washings  added  to  the  contents  of  the  evaporating  dish,  and  the 
latter  put  into  a  draught  at  about  300  C,  till  the  ether  has  disap- 
peared. 
The  contents  of  the  dish  are  poured  into  a  100  c.c.  flask,  the  dish 
washed,  the  washings  added  in  the  flask  and  the  latter  filled  up  to 
the  100  c.c.  mark.  The  solution  containing  hydrastine  sulphate, 
and  of  which  every  10  c.c.  represent  1  gramme  of  the  root,  is  used 
for  the  estimation  of  hydrastine. 
For  the  iodometric  estimation  20  c.c.  of  the  filtered  solution  (rep- 
resenting 2  grammes  of  the  drug)  are  run  from  a  burette  into  a  100 
c.c.  flask  containing  20  or  30  c.c.  of  a  standardized  solution  of  iodine 
of  any  known  strength  (that  in  the  neighborhood  of  1  per  cent,  is 
the  best)  and  the  analysis  carried  out  exactly  as  described  in  our 
previous  paper.1  From  the  amount  of  iodine  consumed  the  amount 
of  hydrastine  is  deduced  by  using  the  factor  of  the  hydrastine  hex- 
iodide,  u  e.  0-60403  of  hydrastine  for  one  of  iodine  consumed. 
For  a  gravimetric  estimation  another  portion  of  20  c.c.  of  the 
filtered  solution  is  run  into  a  separator  and  the  hydrastine  shaken 
out  with  benzol  and  ammonia,  all  the  coloring  matter  remaining  in 
the  aqueous  fluid,  and  a  perfectly  colorless  solution  of  hydrastine  in 
benzol  is  obtained.  The  benzol  solution  is  then  filtered  through  a 
small  filter  into  another  separator,  the  first  separator  and  filter 
washed  with  benzol  and  the  hydrastine  again  shaken  out  with  water 
acidulated  with  sulphuric  acid.    At  last,  from  the  watery  solution 
1  Proc.  Am.  Phar.  Assoc.,  4.6,  368  ;  /.  Am.  Chem.  Soc,  1898,  722. 
