Am.  Jour.  Pharru. 
Aug.,  1893. 
Determination  of  Hydrastine. 
375 
preparations.  In  the  American  Druggist  for  1885,  page  84,  is  a 
paper  by  W.  Simonson  on  the  estimation  of  hydrastine  in  fifty 
samples  of  powdered  hydrastis.  The  method  employed  by  him 
consisted  in  expelling  the  alcohol  from  two  fluidounces  of  tincture 
representing  sixty  grains  of  drug,  adding  water  to  separate  oil, 
resin,  etc.,  and  precipitating  the  crude  alkaloid  from  the  filtered 
solution  with  ammonia.  This  precipitate  he  collected  on  a  filter, 
washed,  dried  and  after  weighing  washed  with  hydrochloric  acid 
and  water  until  nothing  more  was  dissolved,  when  after  again  dry- 
ing and  weighing  the  difference  was  taken  as  alkaloid.  The  average 
yield  from  the  fifty  samples  operated  upon  by  him  was  -125  per 
cent. 
Having  occasion  to  investigate  a  certain  lot  of  fluid  extract  of 
golden  seal  the  writer  made  a  number  of  experiments,  during  which 
it  was  found  that  the  addition  of  a  small  amount  of  ammonia  to  the 
fluid  extract  caused,  after  some  time,  the  separation  of  hydrastine  is 
well  defined  and  remarkably  pure  crystals,  but  unfortunately  accom- 
panied by  a  dark  flocculent  precipitate  that  would  on  the  filter 
accumulate  into  a  compact  mass  very  difficult  to  wash  free  of  alka- 
loid. In  following  up  this  clue  numerous  attempts  were  made  to 
avoid  the  precipitation  of  this  dark  substance  without  success.  But 
the  experiments  developed  a  number  of  interesting  facts. 
It  was  found  first,  that,  by  observing  proper  conditions,  the  alka- 
loid could  be  obtained  in  comparatively  large,  acicular  and  nearly 
colorless  crystals  directly  from  the  fluid  extract. 
Second,  that  the  presence  of  ether  in  quantity  sufficient  to  satu- 
rate the  mother-liquor  very  much  assists  crystallization  and 
enhances  the  purity  of  the  product. 
Third,  that,  if  the  fluid  extract  be  heated  before  adding  the  pre- 
cipitant, a  larger  yield  of  crystals  is  obtained. 
Fourth,  that  the  crystals  can  readily  be  separated  from  the 
accompanying  flocculent  precipitate  by  passing  the  liquid  through  a 
pellet  of  cotton  loosely  inserted  in  the  neck  of  a  funnel.  The  long 
needle-shaped  crystals  of  alkaloid  become  entangled  and  are  retained 
while  the  finely  divided  precipitate  is  permitted  to  wash  through. 
Fifth,  that  the  presence  of  20  to  25  per  cent,  by  volume  of 
officinal  alcohol  is  necessary  in  order  to  secure  good  crystals,  and 
Sixth,  that  a  good  fluid  extract  of  golden  seal  should  yield  from 
1*5  to  2  per  cent,  of  crystallized  white  alkaloid. 
