Am.  Jour.  Pharm 
September,  1899. 
}    British  Pharmaceutical  Conference. 
447 
great  difficulty  with  which  the  separations  take  place,  even  when  the  separator 
is  immersed  in  hot  water.  After  giving  this  process  a  fair  trial  and  experi- 
menting further,  the  authors  decided  to  abandon  it  and  to  adopt  the  following  : 
(4)  Process. — Place  10  c.c.  of  liquid  extract  in  a  basin  over  a  warm  water- 
bath  until  the  alcohol  is  dissipated.  The  solution  is  transferred  to  a  50  c.c. 
flask,  and  the  basin  is  washed  with  small  portions  at  a  time  of  a  mixture  of 
2  c.c.  of  diluted  sulphuric  acid  and  30  c.c.  of  water.  The  solution  is  filtered 
and  water  passed  through  the  filter  until  the  volume  measures  50  c.c.  Of  the 
nitrate  25  c.c,  representing  5  c.c.  of  liquid  extract,  is  transferred  to  a  sepa- 
rator, together  with  the  small  portions  of  water  used  for  washing  the  measure, 
and  the  solution  is  shaken  up  with  10  c.c.  of  chloroform.  After  removal  of 
the  separated  chloroform,  the  solution  is  agitated  with  another  10  c.c.  of  chloro- 
form, which,  after  separation,  is  also  withdrawn.  The  solution  is  then  made 
alkaline  with  ammonia  and  extracted  successively  with  3  X  10  c.c.  of  chloro- 
form. The  chloroform  solutions  are  mixed,  evaporated  and  the  residue 
N 
weighed  and  titrated  with  —  HC1. 
The  accuracy  of  this  process  is  shown  in  an  appended  table,  which  gives 
strictly  comparable  results  on  the  same  sample  of  liquid  extract.  An  addi- 
tional recommendation  is  the  rapidity  with  which  the  assay  can  be  made.  Its 
distinctive  feature  is  the  removal  of  the  resinous  substances  by  a  rapid  and 
simple  method  without  loss  of  alkaloid,  thereby  making  possible  the  quick 
separation  of  the  chloroformic  solutions. 
TABLE  III.— COMPARATIVE  RESULTS. 
Process. 
Amount  of 
Liquid  Extract 
Taken  in  C.c. 
Weight  of 
Alkaloid 
Obtained. 
C.c.  of 
Nic 
HC1 
Absorbed. 
Yield  of 
Alkaloid 
by 
Titration. 
Amount 
of 
Impurity. 
Alkaloid  ir 
per  100  C 
Exti 
By. 
Weighing. 
Grammes 
c.  Liquid 
•act. 
By 
Titration. 
B.P.,  1898  .  . 
20 
•  0*402 
14*0 
Q'3374 
0-0646 
2-010 
1-687 
Wilson's  .  . 
20 
0-400 
13*5 
0-32535 
0-07465 
2-000 
1-62675 
Lime  .... 
5 
0-088 
2-8 
0^06748 
0-02052 
1760 
1*3496 
Kieselguhr  . 
5 
0*106 
4-0 
0-0964 
0-0096 
2T20 
1-928 
No  3  ...  • 
5 
0-114 
4'2 
0-IOI22 
0-01278 
2-28 
2-0244 
No.  4  ...  . 
5 
O'lIO 
4"i 
0-09881 
0-01119 
220 
1-9782 
In  the  above  examinations  the  separations  in  most  cases  were  troublesome, 
owing  to  the  liquid  extract  being  very  resinous. 
The  calculations  are  made  upon  the  basis  that  1  c.  c. 
N 
of-—  HC1  is  equiva- 
lent to  0-0241  gramme  of  mixed  alkaloids,  titration  being  conducted  as  given 
in  the  B.P.,  1898,  page  104,  under  belladonna  assay. 
As  alkaloidal  residues  differ  in  their  degrees  of  purity,  we  are  of  opinion 
that  their  amount  should  not  be  determined  by  gravimetric  processes,  but  that 
their  titration  should  be  insisted  on. 
