Am.  Jour.  Pharra.) 
August,  1908.  / 
Assay  of  Belladonna  Root. 
369 
ether  and  chloroform  can  properly  mix  with  the  powdered  root,  and 
then  add  10  grammes  of  10  per  cent,  ammonia  and  shake  the  flask 
well  at  frequent  intervals  during  an  hour.  The  ammoniacal  liquid 
will  be  entirely  absorbed  by  the  powdered  root,  while  the  alkaloids 
and  resinous  constituents  pass  into  the  ether-chloroform  solution. 
Add  15  c.c.  of  distilled  water  and  shake  the  flask  again  strongly  for 
some  time.  By  this  addition  of  water,  the  powdered  root  separates 
entirely  from  the  solution  in  the  form  of  a  paste,  so  that  either 
through  a  paper  or  a  pellet  of  cotton  100  grammes  of  the  ether- 
chloroform  solution  can  be  transferred  to  a  small  flask.  These  100 
grammes  now  contain  all  that  is  soluble  out  of  10  grammes  of  the 
root.  The  small  flask  is  immersed  in  boiling  water  untilthe  ether 
and  chloroform  are  evaporated,  then  a  few  cubic  centimeters  of  ether 
are  added,  and  this  evaporated  to  be  sure  that  no  ammonia  re- 
mains. The  residue  is  then  dried  for  about  twenty  minutes  in  a 
water  oven  to  remove  every  trace  of  ether,  chloroform  or  ammonia. 
"  In  this  flask  we  now  have,  aside  from  the  total  alkaloids,  a  small 
amount  of  very  light  yellow  or  white  resins,  which,  however,  do  not 
interfere  in  any  way  with  the  following  titrimetric  determination  of 
the  alkaloids  as  the  resins  remain  insoluble  in  the  flask.  To  deter- 
mine the  alkaloid,  put  into  the  flask,  while  yet  warm,  10  c.c.  of  absolute 
alcohol  and  heat  gently  until  everything,  with  the  exception  of  traces 
of  resin,  is  dissolved.  Add  50  c.c.  of  water  and  several  drops  ot 
aqueous  haematoxylin  solution.  The  turbidity  brought  about  by 
resin  contained  in  the  flask  is  of  no  consequence.  However,  I  (Dr. 
Enoch)  add  a  pretty  large  quantity  of  aqueous  haematoxylin  solu- 
tion, which  causes  the  color  to  change  immediately  to  a  deep  red- 
violet  shade.  I  then  add  tenth  normal  hydrochloric  acid  by  drops. 
The  color  changes  very  soon  into  yellow ;  however,  this  is  not  yet 
the  final  point  of  the  titration;  for  after  close  examination,  you  will 
find  that  each  additional  drop  of  acid  still  causes  yellow  streaks  to 
appear  in  the  fluid,  this  being  a  proof  that  the  red  color  of  the 
indicator  has  not  all  been  changed  into  yellow.  I  continue  to  add 
tenth  normal  acid  by  drops  until  the  last  drop  will  no  longer  cause 
any  clarification  nor  any  formation  of  streaks.  The  titration  must 
be  carried  until  this  point  is  reached.  This  point  appears  and  may 
be  determined  so  absolutely  that  I  have  obtained  innumerable  results 
which  coincide. 
"  Multiply  the  number  of  cubic  centimeters  of  tenth  normal 
