462 
Alkaloidal  Assays. 
/Am.  Jour.  Pharm. 
X     October,  1899. 
DIRECTIONS  FOR  CERTAIN  ALKALOIDAL  ASSAYS.1 
By  H.  M.  Gordin  and  A.  B.  Prescott. 
A  General  Method  for  the  Extraction  of  Alkaloids  in  Assays. 
I.  AS  A  METHOD  BY  PERCOLATION.2 
One  to  four  grammes  of  the  finely  powdered  drug  is  weighed 
into  a  low  wide-mouthed  vessel,  with  a  round  bottom,  holding  8  or 
io  ounces,  and  having  a  well-fitted  cork,  such  as  a  screw-top  ointment 
jar.3  The  powder  is  rubbed  up  with  a  small  pestle  to  a  fine  paste, 
by  adding  a  little  of  a  solvent  mixture,  composed  of  stronger  ammo- 
nia water  and  alcohol,  each  5  c.c,  chloroform,  10  c.c,  and  ether,  20 
c.c.4  Then  a  few  more  cubic  centimeters  of  this  mixture  are  added, 
so  as  to  have  the  drug  well  covered  with  the  liquid,  using  in  all 
about  five  times  the  amount  of  the  drug  taken.  The  vessel  is 
corked,  with  the  pestle  inside,  and  is  set  aside  for  about  four  or  five 
hours,  taking  care  to  agitate  by  circular  movement  very  frequently 
during  that  interval.  After  that  time  the  cover  is  removed,  and  the 
vessel  kept  in  a  current  of  air,  stirring  frequently  till  all  odor  of 
ammonia  has  disappeared.  With  a  good  draught  and  frequent 
stirring,  the  powder  will  be  almost  perfectly  dry  in  about  one  hour. 
The  vessel  is  then  put  into  a  vacuum  desiccator  over  sulphuric  acid 
for  about  four  or  five  hours. 
1  In  the  work  of  Research  Committee  D,  Section  2,  Committee  on  Revision 
and  Publication  of  the  Pharmacopoeia  of  the  United  States,  1 890-1 900.  Read 
at  the  meeting  of  the  American  Pharmaceutical  Association,  September,  1899. 
2  These  directions  were  published,  nearly  as  here  given,  by  the  authors,  in  an 
article,  "Emetine  Octoiodide,''  etc.,  Pharm.  Review,  Vol.  17,  1899.  This  gene- 
ral method  is  not  applicable  to  Ipecacuanha.  See  under  "Assay  of  Ipecacu- 
anha," further  on. 
3  An  ordinary  teacup  fitted  with  a  specie  cork  answers  well. 
4  In  the  case  of  Hydrastis  canadensis  the  chloroform  is  replaced  by  an  equal 
volume  of  ether. 
NOTE. — Analytical  results  in  support  of  these  directions  were  given 
in  an  accompanying  paper,  "  Further  Work  Upon  the  Estimation  of  Alka- 
loids and  the  Assay  of  Alkaloidal  Drugs,"  presented  to  this  Association  at  the 
same  date.  Also,  in  the  paper  entitled  "  Certain  Alkaloidal  Periodides,  and  the 
Volumetric  Estimation  of  Alkaloids  as  Higher  Periodides,"  by  the  same 
authors,  "  Proc.  Am.  Phar.  Assoc.,"  1898,  p.  340;  Pharm.  Arch.,  I,  p.  121; 
Jour.  Am.  Chem.  Soc.,  1898,  p.  724.  A  paper  on  "Hydrastine  Hexiodide  and 
Assay  of  Hydrastis,"  Am.  Jour.  Pharm.,  1899,  p.  257.  Further,  see  the  article 
"The  Periodides  of  the  Alkaloids  as  Molecular  Forms  for  Estimation,"  etc., 
by  A.  B.  Prescott,  1897,  Pharm.  Review,  Vol.  15,  and  other  papers  since  1895. 
