154 
Annatto. 
f  Am.  Jour.  Pharm 
\     March,  1886. 
considerably  from  this,  and  though  it  may  not  be  true,  as  some  hint,  that  manu- 
facturing in  this  industry  is  simply  a  term  synonymous  with  adulterating,  yet 
results  will  afterwards  be  given  tending  to  show  that  there  are  articles  in  the 
market  which  have  little  real  claim  to  the  title.  I  tried,  but  failed,  to  procure 
a  sample  of  raw  material  on  which  to  work  with  a  view  to  learn  something  of 
its  character  and  properties  in  this  state,  and  thus  be  able  to  contrast  it  with 
the  manufactured  or  commercial  article.  The  best  thing  to  do  in  the  circum- 
stances, I  thought,  was  to  operate  on  the  highest  priced  sample  at  disposal,  and 
this  was  done  in  all  the  different  ways  that  suggested  themselves.  The  extrac- 
tion of  the  resin  by  means  of  alcohol — the  usual  way,  I  believe — was  a  more 
troublesome  operation  than  it  appeared  to  be,  as  the  following  experiment  will 
show:  One  hundred  grains  of  No.  8  were  taken,  dried  thoroughly,  reduced  to 
fine  powder,  and  introduced  into  a  flask  containing  4  ounces  of  alcohol  in  the 
form  of  methylated  spirit,  boiled  for  an  hour — the  flask  during  the  operation 
being  attached  to  an  inverted  condenser — filtered  off,  and  the  residue  treated 
with  a  smaller  amount  of  the  spirit  and  boiled  for  ten  minutes.  This  was  re- 
peated with  diminishing  quantities  until  in  all  14  ounces  had  been  used  before 
the  alcoholic  solution  ceased  to  turn  blue  on  the  addition  to  it  of  strong  sul- 
phuric acid,  or  failed  to  give  a  brownish  precipitate  with  stannous  chloride.  As 
the  sample  contained  a  considerable  quantity  of  potassium  carbonate,  in  which 
the  resin  is  soluble,  it  was  thought  that  by  neutralizing  this  it  might  render  the 
resin  more  easy  of  extraction.  This  was  found  to  be  so,  but  it  was  accompanied 
by  such  a  mass  of  extractive  as  made  it  in  the  long  run  more  troublesome,  and 
hence  it  was  abandoned.  Thinking  the  spirit  employed  might  be  too  weak,  an 
experiment  with  commercial  absolute  alcohol  was  carried  out  as  follows :  One 
hundred  grains  of  a  red  sample,  No.  4,  were  thoroughly  dried,  powdered  finely, 
and  boiled  in  2  ounces  of  the  alcohol,  filtered,  and  the  residue  treated  with  half 
an  ounce  more.  This  required  to  be  repeated  with  fresh  half  ounces  of  the 
alcohol  until  in  all  7 i  were  used,  the  time  occupied  from  first  to  last  being 
almost  three  hours.  This  was  considered  unsati ^factory,  besides  being  very 
expensive,  and  so  it,  also,  was  set  aside,  and  a  series  of  experiments  with 
methylated  spirit  alone  was  set  in  hand.  The  results  showed  that  the  easiest 
and  most  satisfactory  way  was  to  take  100  grains  (this  amount  being  preferred 
as  it  reduces  error  to  the  minimum),  dry  thoroughly,  powder  finely,  and  macer- 
ate with  frequent  agitation  for  twenty-four  hours  in  a  few  ounces  of  spirit,  then 
to  boil  in  this  spirit  for  a  short  time,  filter,  and  repeat  the  boiling  with  a  fresh 
ounce  or  so ;  this,  as  a  rule,  sufficing  to  completely  exhaust  it  of  its  resin.  Wyn- 
ter  Blyth  says  that  the  red  resin,  or  bixin,  is  soluble  in  25  parts  of  hot  alcohol. 
It  appears  from  these  experiments  that  much  more  is  required  to  dissolve  it  out 
of  commercial  annatto. 
The  full  process  followed  consisted  in  determining  the  moisture  by  drying 
100  grains  at  212°  F.  till  constant,  and  taking  this  dried  portion  for  estimation  of 
the  resin  in  the  way  just  stated.  The  alcoholic  extract  was  evaporated  to  dry- 
ness over  a  water-bath,  the  residue  dissolved  in  solution  of  sodium  carbonate 
and  the  resin  precipitated  by  dilute  sulphuric  acid  (these  reagents  being  chosen 
as  the  best  after  numerous  trials  with  o*  hers),  added  in  the  slightest  possible 
excess.  The  resin  was  collected  on  a  tared  double  filter  paper,  washed  with 
distilled  water  until  the  washings  were  entirely  colorless,  dried  and  weighed. 
The  ash  was  found  in  the  usual  way,  and  the  extractive  by  the  difference.  In 
