Am.  Jour.  Pharm. 
Aug.,  1893. 
} 
Determination  of  Hydrastine. 
377 
The  crystals  cannot  well  be  collected  on  a  filter  for  the  impurity 
spoken  of  above,  which  is  simultaneously  precipitated,  will  also  be 
retained  and  necessitate  a  second  or  even  third  crystallization.  The 
use  of  cotton  obviates  this.  A  little  practice,  however,  is  necessary 
in  preparing  the  funnel.  If  the  cotton  plug  is  inserted  too  tightly  it 
will  soon  clog  and  render  thorough  washing  impossible,  if  too  loose 
alkaloid  may  pass  through.  Very  naturally  the  cotton  retains  some 
coloring  matter,  but  this  can  be  ignored  as  it  never  amounts  to  more 
than  a  few  milligrammes  and  does  not  introduce  any  appreciable 
error. 
If  it  is  desired  to  determine  the  amount  of  berberine  also  it  can, 
by  appropriate  treatment,  be  obtained  from  the  mother-liquor  of 
hydrastine  determination,  but  the  order  cannot  with  advantage  be 
reversed,  because  when  the  fluid  has  once  been  treated  with  acids 
to  precipitate  berberine  salts  the  hydrastine  obtained  from  it  is 
very  impure  and  also  more  difficult  to  purify. 
An  alternative  process  of  assay,  which,  however,  requires  more 
attention,  consists  in  rendering  25  cc.  of  fluid  extract  alkaline  with 
ammonia  and  rotating  in  a  separator  with  three  separate  portions 
of  ether  of  15  cc.  each,  extracting  the  alkaloid  from  the  mixed 
ether  washings  by  agitating  them  with  three  portions  of  10  cc.  each 
of  2  per  cent,  sulphuric  acid,  and  lastly  with  5  cc.  of  distilled  water, 
adding  to  the  combined  washings  10  cc.  of  alcohol,  3  cc.  of  ether 
and  ammonia  sufficient  to  render  alkaline.  After  allowing  to  stand 
for  six  hours  with  frequent  agitation,  the  crystals  are  collected, 
dried  and  weighed. 
Shaking  Out 
Precipitation. 
Alkaloid 
from  25  cc. 
Percent,  of 
alkaloid. 
Alkaloid 
from  25  cc. 
Percent,  of 
alkaloid. 
r 
•447 
•455 
1788 
1-82 
•458 
•443 
•442 
•445 
•485 
•582 
1 -83 
177 
1768 
178 
1-  941 
2-  328 
Fluid  Extract  No.  22907  - 
Fluid  Extract  No.  2291 1 
1  This  result  was  obtained  after  the  fluid  extract  had  stood  for  several  days  in  a  loosely 
covered  vessel. 
