Am'iug.%?9b3arm"}  Hydrastis  Canadensis.  371 
Golden  Seal  contains  three  alkaloids,  namely,  berberine,  C.^Hj 
N04;  hydrastine,  C21H21N06,  and  canadine,  C21H21N04,  the  latter 
having  been  in  dispute  for  some  time,  and  its  presence  but  recently 
established  by  F.  Wilhelm  and  E.  Schmidt.  Canadine  is  present, 
however,  in  but  small  quantities  and,  therefore,  may  be  ignored  in 
the  estimation  of  berberine  and  hydrastine.  The  most  important 
constituent  of  this  drug  is  its  hydrastine  based  on  the  medical 
reports,  and  it  is  this  on  which  we  are  to  judge  of  the  quality  of  the 
drug  or  any  preparation  made  from  it. 
ASSAY  OF  THE  DRUG. 
Ten  grams  of  the  drug  in  a  moderately  fine  powder  is  exhausted 
with  strong  alcohol  by  hot  re-percolation,  requiring  2  or  3  hours, 
percolate  cooled  and  diluted  to  100  cc.  with  same  menstruum,  25 
cc.  of  this  tincture  is  placed  in  a  suitable  flask,  1-3  cc.  HC1,  U.  S.  P., 
0-2  cc.  H2S04,  and  12-5  cc.  concentrated  ether  added  and  the 
mixture  allowed  to  stand  24  hours  in  a  cool  place,  with  frequent 
shaking.  At  the  end  of  this  time  transfer  the  crystals  to  counter- 
poised filter  papers,  washing  them  with  a  mixture  of  equal  volume 
of  concentrated  ether  and  strong  alcohol  until  filtrate  gives  no  acid 
reaction.  Dry  crystals  at  1050  C,  weigh,  and  multiply  weight  by 
0-9017  to  obtain  the  amount  of  berberine  alkaloid,  and  then  multi- 
ply this  result  by  40  to  ascertain  the  percentage. 
The  filtrate  from  berberine  estimation  is  rendered  nearly  neutral, 
evaporated  to  a  small  volume,  solution  cooled  and  transferred  to  a 
separator  and  the  residue  remaining  in  evaporating  dish  is 
thoroughly  washed  with  slightly  acidulated  water  till,  free  from 
alkaloid,  the  washings  added  to  the  separator.  Render  fluid  alka- 
line with  ammonia  water  and  extract  the  alkaloid  with  several 
portions  of  chloroform,  evaporating  the  chloroformic  solution  to 
dryness  at  a  low  heat,  protected  from  light.  Redissolve  in  acid 
water,  transfer  to  2  oz.  prescription  vial,  wash  with  ether,  reject- 
ing the  same.  Reprecipitate  alkaloid  with  ammonia  water  and 
extract  with  several  portions  of  ether.  Evaporate  the  ethereal 
solutions  in  a  shallow  crystallizing  dish.  Now  dissolve  the  residue 
in  10  cc.  H2S04  (a  small  amount  of  ether  facilitates  the  solution 
of  the  alkaloids)  add  20  or  30  cc.  water,  2  drops  of  cochineal  tinc- 
ture 1  :  10  and  determine  the  free  acid  by  titration  with  N-ioo 
sodium  hydrate  solution.    Each  cc.  of  N-ioo  H2S04  neutralized 
