Am.  Jour.  Pharm. \ 
January,  1901.  J 
Assay  of  Belladonna  Root. 
23 
More  important  than  all  these  considerations  is  the  fact  that,  on 
account  of  the  concentrated  character  of  the  menstruum  used,  there 
is  very  little  inert  resinous  matter  carried  through,  and  consequently 
the  shaking-out  part  of  the  assay  is  free  from  this  serious  complica- 
tion, always  present  in  assaying  an  ordinary  extract.  Presumably, 
because  of  this  feature,  emulsification  of  the  alkaline  solution  is 
quite  infrequent  instead  of  being  the  rule,  as  in  assaying  an  extract. 
METHOD  OF  PROCEDURE. 
Weigh  out  in  a  tared  beaker  about  20  grammes  of  the  root 
ground  moderately  fine.  It  is  not  necessary  to  weigh  closer  than 
the  third  decimal  place  in  grammes,  as  an  error  of  -00 1  gramme 
here  is  not  appreciable  in  the  percentage  result.  Pour  the  weighed 
contents  of  the  beaker  carefully  into  a  clean,  smooth  porcelain  dish, 
of  1 8  or  20  centimetres  diameter,  tapping  the  beaker  to  shake  out 
as  much  of  the  root  as  possible. 
The  menstruum  used  is  that  advised  by  Dunstan  and  Ranson,  and 
is  manipulated  as  follows :  Mix  up  6o  c.c.  or  70  c.c.  of  equal  parts 
by  volume  of  absolute  alcohol  and  chloroform,  and  take  about  one- 
quarter  of  the  mixture  to  moisten  the  root  in  the  porcelain  dish. 
Pour  this  portion  of  the  alcohol-chloroform  mixture  first,  into  the 
tared  beaker,  whirling  it  around  to  collect  the  fine  particles  of  root 
which  adhered  to  the  glass,  then  pour  it  into  the  dish  and  mix  up 
well  with  a  clean  spatula  until  the  root  is  evenly  moistened. 
Now  take  the  inside  glass  cup  of  the  reflux  extractor,  which 
should  be  about  I  inch  in  diameter  and  3  inches  deep,  put  in  the 
bottom  an  absorbent  cotton  plug  moistened  with  the  alcohol-chloro- 
form mixture  and,  holding  the  cup  over  the  dish  so  as  to  catch  in 
the  latter  any  that  falls,  carefully  transfer  with  a  spatula  a  little  root 
at  a  time  into  the  cup,  packing  it  in  gently  with  a  large,  smoothly- 
rounded  glass  rod,  finally  shaking  off  any  particles  of  root  adhering 
to  the  rod  and  spatula. 
Prepare  a  small  wad  of  absorbent  cotton  for  the  top  of  the 
packed  root,  moisten  it  with  some  of  the  mixture  and  use  one  side 
of  it  as  a  mop  to  take  up  the  last  particles  of  the  moistened  root 
from  the  porcelain  dish,  spatula  and  rod. 
Now  place  this  cotton  on  top  of  the  root  packed  in  the  glass  cup, 
putting  the  side  downwards  that  was  used  as  a  mop. 
On  top  of  the  whole  place  sufficient  clean  lead  shot  to  cover  it 
and  to  hold  it  down. 
