716 
Atropine  Sulphate 
( Am.  Jour,  Pharm. 
(       Oct.,  1921, 
lots  ranged  from  33.98%  to  93.06%,  the  larger  amounts  being  re- 
covered when  larger  proportions  (359  pounds  to  5000  gallons,  rep- 
resenting 15,500  pounds  green  Stramonium)  of  the  reagent  was 
added. 
The  adsorbed  alkaloids  were  recovered  by  extraction  with  ether 
after  making  alkaline. 
The  reagent,  after  extraction,  always  contained  about  0.2  per 
cent,  of  alkaloid,  which  could  not  be  economically  removed. 
Experiments  in  which  other  acids  were  used  to  facilitate  ex- 
traction showed  no  marked  differences  from  those  recorded,  although 
other  preservatives,  such  as  bleaching  powder,  cresol,  and  sodium 
bisulphite,  gave  better  results  than  formaldehyde  in  the  matter  of 
the  yield  of  alkaloid. 
The  crude  alkaloidal  material  recovered  from  the  "reagent"  was 
purified  as  follows : 
PURIFICATION  OF  THE  CRUDE  ATROPINE. 
The  alkaloidal  material  was  extracted  from  the  Lloyd's  reagent 
with  95  per  cent,  alcohol,  using  lime  to  obtain  the  proper  alkalinity. 
The  extractions  were  acidulated  with  acetic  acid  and  the  solution 
concentrated  first  to  12  per  cent.,  and  then  under  diminished 
pressure  to  2  per  cent,  of  its  original  volume.  This  procedure  was 
sufficient  to  convert  all  the  hyoscyamine  into  atropine.  After  neu- 
tralization with  ammonia,  the  solution  was  allowed  to  stand  over 
night  and  filtered.  A  test  portion  of  the  filtrate  was  shaken  with 
ether.  If  an  emulsion  resulted,  the  solution  was  diluted  about  one- 
fourth  and  returned  to  the  vacuum  still.  Distilling  the  neutral  li- 
quid, and  again  filtering,  usually  prevented  the  troublesome  emulsion 
with  ether.  Ammonia  was  added  until  the  solution  was  alkaline  and 
the  atropine  alkaloid  extracted  with  ether.  After  evaporation  of  the 
ether,  the  alkaloid  was  carefully  dried  at  about  35 0  C. 
The  dried  alkaloid  was  dissolved  in  ethyl  alcohol  in  the  propor- 
tion of  one  ounce  of  alkaloid  to  two  fluid  ounces  of  solvent,  and  the 
solution  almost  neutralized  with  sulphuric  acid,  using  cochineal  as  in- 
dicator. After  filtering  it  was  evaporated  on  the  water  bath  to  a 
thin  sirup,  and  to  this  sirup,  while  still  warm,  acetone  was  added 
almost  to  the  point  of  precipitation  of  the  atropine  sulphate. 
On  cooling,  the  atropine  sulphate  crystallized.   If  not  sufficiently 
