Am.  Jour.  Pharm.  \ 
October,  1914.  j 
Analyses  of  Tzvo  Echinacea  Roots. 
455 
oil  separated  in  the  usual  manner  weighed  1.4  Gm.  It  was  amber 
colored  and  had  a  powerful  odor.  This  is  equivalent  to  0.04  per 
cent,  of  the  air-dried  drug. 
The  resin,  to  which  the  medicinal  properties  are  ascribed,  was 
prepared  from  a  quantity  of  the  fresh  drug,  corresponding  to  33.3 
kilogrammes  of  air-dried  drug.  This  drug  was  exhausted  by  per- 
colation with  alcohol,  the  percolate  (260  litres)  was  concentrated  by 
distillation  under  diminished  pressure  to  a  volume  of  1 1.5  litres.  This 
concentrated  alcoholic  solution,  from  which  a  fatty  layer  separated 
in  considerable  quantity,  was  mixed  with  about  20  litres  of  distilled 
water,  whereupon  the  precipitation  of  the  resin  was  complete.  After 
continued  agitation  for  the  purpose  of  thoroughly  washing  the  resin, 
and  long  standing,  the  resin  separated  above  a  clear,  reddish-brown 
aqueous  layer.  By  siphoning,  most  of  the  aqueous  layer  could  be 
separated  from  the  resin.  It  was  noticed  that  a  very  slight  inter- 
mediate zone  between  the  resin  layer  and  the  aqueous  layer  con- 
tained crystalline  material.  This  was  separated  by  mechanical 
means  and  in  very  small  quantity,  and  crystallized  from  95  per  cent, 
alcohol.  It  proved  to  be  an  impure  phytosterol,  crystallizing  in  the 
characteristic  laminae,  melting  at  about  131 0  to  1360  indefinitely,  and 
giving  the  usual  color  reactions.   It  was  returned  to  the  resin. 
The  resin  was  finally  washed  with  water,  taken  up  in  alcohol, 
and  then  dried  in  a  vacuum.  The  weight  was  628  Gm.,  equivalent  to 
1.88  per  cent.  It  is  a  brownish-yellow  resin,  and  if  dissolved  in 
alcohol  forms  an  amber-colored  solution,  which  yields  no  crystalline 
deposit.  It  is  possible,  however,  to  obtain  in  the  first  fraction  a  green 
resinous  deposit,  which  differs  from  the  resin  proper,  which  has  the 
characteristic  taste  of  the  root.  The  material  was  brought  into  one 
fraction,  taken  up  in  purified  sawdust,  and  extracted  with  the  follow- 
ing results : 
Gramme. 
Ligroin  extract    222.0 
Ether  extract   107.0 
Chloroform  extract   180.0 
Ethyl  acetate  extract    35.0 
Alcohol  extract    70.0 
Total    614.0 
We  are  studying  these  extracts  as  well  as  the  water-soluble  ex- 
tract in  more  detail. 
Chemical  Research  Laboratory,  The  Upjohn  Company, 
Kalamazoo,  Michigan. 
