io8 
Assay  of  Belladonna  Leaves. 
(Am.  Jour.  Phariu. 
\      March,  1899. 
portions.  A  fifth  portion  of  20  c.c.  ether-chloroform  was  used  in 
a  number  of  assays  to  determine  if  the  alkaloids  were  perfectly 
extracted  by  the  preceding  four  portions  of  solvent,  but  in  no 
case  did  the  residue  obtained  cause  an  alkaline  reaction  with  the 
indicator. 
The  assay  of  the  leaves  therefore  was  conducted  as  follows : 
Moisture  determined  in  a  separate  portion  of  2  grammes  at  ioo° 
Assay  Proper. — Twenty  grammes  of  the  powdered  leaves  were 
placed  in  a  glass-stoppered  bottle  of  250  c.c.  capacity,  tared,  100 
grammes  ether  and  25  grammes  chloroform  added ;  after  several 
minutes'  agitation  10  c.c.  ammonia  water  (10  per  cent.)  were  added, 
and  the  mixture  frequently  agitated  during  one  to  two  hours  ;  after 
adding  4.0  c.c.  H20  agitate  thoroughly  for  several  minutes  ;  set 
aside  for  ten  minutes,  and  pour  off  as  much  as  possible  of  the  ether- 
chloroform  solution  into  a  clean,  dry  flask  ot  about  1 50  c.c.  capacity. 
Weigh  this  flask  with  contents,  and  after  standing  about  one-half 
hour  (to  allow  any  drug  and  aqueous  solution  which  may  be  carried 
over,  to  separate),  pour  into  a  separating  funnel  as  much  as  possible 
of  the  clear  ether-chloroform  solution  and  weigh  the  flask  with  its 
residual  contents.  The  difference  between  the  two  weights  gives  the 
weight  of  the  solution  transferred,  and  represents  a  certain  weight 
of  the  leaves,  the  exact  amount  of  the  latter  being  calculated  by  the 
proportion: 
125  gm.,  wt.  of  solvent  used  :  20  gm.  :  :  wt.  of  transferred  solution  :  x. 
The  ether-chloroform  solution  is  extracted  with  four  portions  of 
acidulated  water  (2  c.c.  H2S04  to  make  500  c.c.)  of  25,  15,  10  and  5 
c.c.  respectively ;  the  first  three  portions  are  collected  in  one  beaker, 
while  the  last  one  is  kept  separately.  After  cleaning  the  separatory 
funnel  the  contents  of  the  beaker  are  returned  and  the  last  portion 
of  5  c.c.  acidulated  water  used  to  rinse  this,  and  also  returned  to  the 
separatory  funnel ;  5  c.c.  water  are  then  used  to  complete  the  rinsing 
of  the  beaker  and  added  to  the  acid  solutions.  The  acid  solution  is 
next  agitated  with  25  c.c.  ether-chloroform  (2  parts  ether  and  3 
parts  chloroform  by  weight),  8  c.c.  ammonia  water  (10  per  cent.) 
added  and  again  thoroughly  agitated ;  after  separation  the  ether- 
chloroform  is  run  into  a  smaller  separator  and  extraction  repeated 
with  15,  10  and  5  c.c.  ether-chloroform;  while  this  last  portion  is 
separating  the  first  three  portions  are  filtered  through  a  small  fil- 
ter, wetted  with  the  solvent  mixture,  into  an  Erlenmeyer  flask  of 
