Am.  Jour.  Pharm.  ) 
September,  1913.  J 
An  Assay  for  Sanguinaria. 
397 
Many  experiments  and  scores  of  unsuccessful  assays  were  neces- 
sary to  determine  the  facts  given  above.  From  them  the  following 
assay  was  evolved : 
Gradually  add  seven  cubic  centimetres  of  water  to  two  grams 
of  air-slaked  lime  contained  in  a  suitable  dish.  To  the  magma  thus 
formed,  add  two  grams  of  finely  powdered  Sanguinaria  and  incor- 
porate thoroughly.  Evaporate  on  a  water  bath  to  dryness.  Trans- 
fer the  dry  material,  after  powdering,  to  a  small  percolator,  the  ori- 
fice of  which  has  been  closed  with  a  pledget  of  paper  pulp,  moist- 
ened with  a  mixture  of  equal  volumes  of  ether  and  benzol.  Rinse 
the  dish  with  a  few  cubic  centimetres  of  the  same  ether-benzol 
mixture  and  pour  the  rinsings  upon  the  material  contained  in  the 
percolator.  Continue  the  percolation  by  the  addition  of  small  por- 
tions of  the  ether-benzol  mixture  from  time  to  time  until  a  drop 
of  the  percolate,  evaporated  in  a  watch  crystal  and  redissolved  by 
the  addition  of  one  drop  of  diluted  Hydrochloric  Acid,  no  longer 
gives  a  precipitate  with  Mayer's  Reagent.  Transfer  the  percolate 
to  a  separatory  funnel  and  wash  with  separate  portions  of  solution 
of  Citric  Acid  (5  per  cent,  of  25  c.c,  15  c.c.  and  10  c.c.  respec- 
tively. Continue  the  treatment  with  portions  of  5  c.c.  of  the  acid 
solution  till  one  drop  of  the  acid  solution  shows  no  precipitate  with 
Mayer's  Reagent.3  Transfer  the  mixed  acid  solutions  to  a  separa- 
tory funnel,  add  15  c.c.  of  Benzol  and  afterwards  sufficient  Sodium 
Hydroxide  Solution  to  make  the  mixture  alkaline  to  Litmus.  Shake 
the  mixture  thoroughly.  Separate  and  filter  the  benzol  layer  into  a 
tared  beaker.  Repeat  the  operation  with  two  portions  of  10  c.c. 
each  of  benzol,  mixing  the  separated  and  filtered  benzol  solutions 
with  that  first  obtained.  Evaporate  the  mixed  solutions,  on  a 
water-bath,  to  dryness.  Cool  the  beaker  and  residue  in  a  desiccator 
and  weigh.  The  commercial  drug  at  present  assays  from  3-4  per 
cent,  total  alkaloid. 
For  assaying  the  Tincture  and  Fluidextract  take  20  c.c.  and 
2  c.c.  respectively  and  evaporate  the  Alcohol  on  a  water-bath;  mix 
with  the  lime  magma  and  proceed  as  above. 
The  residues  given  by  this  method  are  practically  white  and 
crystalline.  Results  are  remarkably  constant  as  compared  with 
previous  assays,  the  weights  rarely  varying  more  than  .001  in 
assaying  the  same  sample. 
3  Total  extraction  of  alkaloid  is  generally  shown  by  absence  of  color  in 
the  Citric  Acid  Solution. 
