446  British  Pharmaceutical  Conference.     {^fSE^fwff ■ 
THE  ASSAY  OF  THE  LIQUID  EXTRACT  AND  WINE  OF 
IPECACUANHA  OF  THE  B.P.,  1898. 
By  W.  A.  H.  Kaylor  axd  Johx  J.  Bryant. 
The  authors  experimented  with  a  number  of  processes,  of  which  the  following 
are  deserving  of  mention. 
(1)  The  Lime  Process. — To  5  grammes  of  slaked  lime  in  a  basin  add  5  c.c.  of 
liquid  extract,  care  being  taken  to  prevent  the  latter  from  coming  into  direct 
contact  with  the  containing  vessel.  The  measure  is  rinsed  with  alcohol  and 
the  rinsings  added  to  the  lime  mixture,  and  the  whole  dried  over  a  water-bath. 
The  dry  residue  is  next  exhausted  in  a  Soxhlet  by  boiling  ether.  The  ethereal 
solution  is  extracted  with  y2  per  cent,  sulphuric  arid,  and  the  latter  with  am- 
monia and  chloroform.  The  residue  from  the  chloroformic  extractions  was 
dried  and  weighed. 
The  only  object  in  including  Glenard's  process  is  to  point  out  the  exact 
cause  of  the  low  results  yielded  by  it.  The  explanation  is  rendered  possible  by 
the  elaborate  researches  of  Paul  and  Cownley  on  ipecacuanha.  Small  quanti- 
ties of  the  alkaloids,  emetine  and  cephaeline  in  a  pure  condition  were  treated 
alone  and  separately  by  the  lime  process  exactly  as  with  the  liquid  extract,  the 
alkaloid  being  first  dissolved  in  alcohol.  The  results  here  tabulated  clearly 
show  that  the  loss  of  alkaloid  is  due  to  the  action  of  the  lime  on  the  cephaeline, 
the  emetine  being  uninfluenced  by  the  treatment. 
TABLE  II.— LIME  PROCESS  WITH  PURE  ALKALOIDS. 
Alkaloid. 
Amount 
Amount 
Per  Cent. 
Per  Cent. 
Taken. 
Returned. 
Returned. 
Loss. 
0"IOO 
o-09S 
93 
2 
Cephaeline  
0074 
o-o6o 
81*09 
18-91 
(2)  Kieselguhr  Process. — To  5  grammes  of  kieselguhr,  freed  from  every  trace 
of  lime,  placed  in  a  porcelain  basin,  add  5  c.c.  of  the  liquid  extract,  and  dry  the 
mixture  over  the  water-bath.  The  dry  powder,  after  transference  to  a  Soxhlet, 
is  then  treated  throughout  by  Ransom's1  ammoniated  chloroform  process.  The 
chief  drawbacks  to  this  method  are  the  time  and  care  required  for  its  exact 
performance. 
(3)  Process. — To  5  c.c.  of  the  liquid  extract,  placed  in  a  porcelain  basin,  add 
two  drops  of  diluted  sulphuric  acid,  and  heat  over  the  water-bath  gently  to 
drive  off  the  spirit.  The  acid  solution  is  then  transferred  to  a  separator, 
together  with  the  small  portions  of  water  used  for  washing  the  basin,  ammonia 
is  added  in  excess,  followed  by  10  c.c.  of  chloroform  and  agitated.  The  agita- 
tion and  separation  with  chloroform  is  twice  repeated.  The  chloroformic  solu- 
tions are  mixed  and  extracted  with  10  c.c.  of  Yz  per  cent,  sulphuric  acid  thrice 
repeated.  The  separated  acid  solutions  are  united,  rendered  alkaline  with 
ammonia  and  extracted  with  three  successive  10  c.c.  of  chloroform.  The 
chloroformic  solutions  are  evaporated  and  the  residue  dried,  weighed  and  ti- 
trated with  1Q  HC1.  Although  the  process  is  not  open  to  the  charge  of  inac- 
curacy, it  has  the  one  serious  defect  of  consuming  much  time,  owing  to  the 
1  "  Year-Book  of  Pharm  ,"  1887,  p.  450. 
