AmMa"'iShrm'}     Contributions  from  H.  M.  Got  din.  217 
II.  ASSAY  OF  CONIUM  SEED  OR  LEAVES. 
The  assay  of  this  drug  presents  considerable  difficulty.  Owing 
to  the  volatility  of  confine  even  at  ordinary  temperature,  its  solu- 
tions in  immiscible  solvents  cannot  be  evaporated  without  loss,  and 
as  the  alkaloid  is  not  completely  precipitated  by  Mayer's  or  Wag- 
ner's reagents,  it  cannot  be  estimated  by  my  general  method.  The 
method  which  I  have  found  to  give  excellent  results  is  a  modifica- 
tion of  the  method  of  Cripps,1  and  its  details  are  as  follows  : 2 
Put  20  grammes  of  finely  powdered  conium  into  a  300  c.c. 
glass-stoppered  bottle,  pour  in  200  c.c.  of  a  previously  prepared 
mixture  of  one  volume  of  chloroform  and  three  volumes  ether, 
shake  about  five  minutes,  add  10  c.c.  liquor  potassa,  shake  fre- 
quently during  four  hours,  and  set  aside  over  night.  Pipette  off 
100  c.c.  of  the  clear  liquid  into  a  300  c.c.  flask,  add  10  c.c.  of  a  2 
per  cent,  solution  of  oxalic  acid  in  alcohol  and  mix  well.  Distil 
off  the  liquid  completely,  removing  the  last  traces  by  blowing  aif 
into  the  flask  while  keeping  it  on  the  water-bath.  Let  cool,  add  10 
c.c.  absolute  alcohol,  warm  gently  and  cool  again.  Filter  the  alco- 
holic solution  into  a  wide  beaker,  washing  the  flask,  and  filter 
three  times  with  5  c.c.  each  time  of  absolute  alcohol.  Evaporate 
the  alcohol  almost  completely  from  a  warm  water-bath,  add  10  c.c. 
water  and  pour  into  a  25  c.c.  measuring  flask,  cool,  and  fill  up  to 
the  mark  with  water.  Add  about  2  grammes  talcum,  shake  well 
and  filter  through  a  small  dry  filter.  Pipette  off  12  5  c.c.  (=  5 
grammes  drug)  into  a  100  c.c.  separator,  add  25  c.c.  petroleum 
ether  (boiling  below  6o°  C.  and  leaving  no  residue  on  evaporation) 
and  5  c.c.  of  a  10  per  cent,  solution  of  KOH.  Shake  well  and  set 
aside  until  the  liquid  separates  into  two  layers.  Draw  off  lower 
layer  into  a  50  c.c.  separator,  add  to  it  20  c.c.  petroleum  ether,  and 
shake.  After  separation  into  two  layers,  draw  off  lower  layer  into 
a  beaker  and  pour  contents  of  second  separator  into  the  first  one. 
Return  the  aqueous  liquid  to  the  smaller  separator  and  shake  it 
again  with  20  c.c.  petroleum  ether.  Draw  off  aqueous  layer  and 
pour  the  petroleum  ether  from  the  second  into  the  first  separator. 
1  Pharm.  J.  Trans.  (3),  18,  13,  511  ;  Allen,  "  Commerc.  Org.  Anal.,"  Vol. 
Ill,  part  II,  1892,  176. 
2  Later  on  I  intend  to  test  the  exactness  of  this  method  by  comparing  its 
results  with  those  obtained  by  some  standard  method  as  given  in  the  previous 
paper. 
