322 
Assay  of  Belladonna  Leaves. 
Am.  Jour.  Pharm. 
July,  1899. 
to  practically  fill  up  the  neck  of  the  percolator;  compress  the  rub- 
ber tubing  with  a  pinch-cock,  to  allow  preparation  for  the  percola- 
tion. Place  20  grammes  of  the  powdered  leaves  in  the  percolator, 
add  50  c.c.  menstruum  [alcohol  (95  per  cent.),  180  grammes;  water 
of  ammonia  (10  per  cent.),  20  grammes]  and  stir  with  a  heavy  iron 
wire  until  a  homogeneous  mixture  results,  and  in  such  a  manner 
that  the  air-bubbles  are  brought  as  completely  as  possible  to  the 
surface;  rinse  the  wire  and  sides  of  the  percolator  with  10  c.c.  of  the 
menstruum  and  allow  percolation  to  proceed  at  once;  add  more 
menstruum  from  time  to  time  in  quantities  of  20  to  30  c.c.  until 
200  c.c.  have  been  used,  allowing  the  portions  to  flow  down  the 
sides  of  the  percolator  to  avoid  stirring  up  of  the  drug.  Collect 
the  first  portions  of  the  percolate,  about  IOO  c.c,  in  a  porcelain  dish 
of  about  150  c.c.  capacity,  and  the  last  portions  in  a  beaker;  place 
the  dish  with  contents  upon  a  water-bath,  the  temperature  of  which 
is  kept  at  from  500  to  6o°  C,  and  as  the  solvent  evaporates  add 
the  weaker  percolate;  continue  heating  until  the  odor  of  alcohol  is 
no  longer  recognizable  after  stirring.  Make  a  mixture  of  05  c.c. 
water  of  ammonia  and  10  c.c.  water  and  use  this  in  portions  of  I  to 
2  c.c.  to  soften  the  extract  and  transfer  it  to  a  separator  (250  c.c. 
capacity),  add  50  c.c.  of  an  ether-chloroform  mixture  (ether  4  parts, 
chloroform  1  part  by  weight)  and  agitate;  now  add  25  c.c.  acidu- 
lated water  (2  c.c.  H2S04,  U.S.P.,  diluted  with  water  to  500  c.c), 
using  this  to  rinse  the  dish  from  which  the  extract  has  been 
removed,  agitate  thoroughly,  and  after  separation  of  the  liquids 
allow  the  acid  solution  to  run  through  a  small  filter  (5-5  cm.  in 
diameter)  into  a  beaker;  repeat  with  15,  10  and  5  c.c.  acidulated 
water.  Collect  the  first  three  portions  together,  reserving  the  last 
portion  to  rinse  the  beaker  containing  the  first  portions;  clean  the 
separator,  introduce  the  acid  solutions,  finally  rinsing  the  beaker 
with  5  c.c  water,  add  25  c.c  chloroform-ether  (chloroform  2  parts, 
ether  1  part  by  weight)  and  8  c.c.  water  of  ammonia  and  agitate 
thoroughly  (should  an  emulsion  form,  proceed  as  described  in  the 
earlier  part  of  this  paper) ;  after  separation  transfer  the  chloro- 
form-ether solution  to  a  smaller  separator  (about  100  c.c  capacity) 
and  repeat  the  extraction  with  15,  10  and  5  c.c.  of  the  solvent; 
while  this  last  portion  is  separating,  run  the  other  portions  through 
a  small  filter  into  a  clean,  dry  flask  of  about  120  c.c  capacity;  rinse 
the  smaller  separator  with  the  last  extraction  and  transfer  to  the 
