VIII. B. 6 DuMcz: Oleoresin of Asindium 531 



served at room temperature, about 30^ C. In each case, with 

 the exception of ether and acetone, the specified quantities of 

 the extract and solvent were placed in a 25 cubic centimeter 

 graduated, glass-stoppered cylinder and thoroughly shaken. The 

 mixture was then cooled for two hours at a temperature of 15° 

 C, and the volume of the oil thus separated was noted. The 

 difference in this volume and that of the original quantity of the 

 extract represents roughly the amount of castor oil when used 

 as an adulterant. Where no castor oil has been added, prac- 

 tically the original volume of the extract was observed. For a 

 more exact determination of the castor oil, when present, the 

 following procedure was carried out. 



Quantitative determination of castor oil. — A weighed quantity 

 of the extract, about 10 grams, was introduced into a separator 

 and shaken with an equal volume of petroleum ether. Part of 

 the petroleum ether was used to aid in transferring all of the 

 extract from the container in which it was weighed to the separ- 

 ator. After shaking, the mixture was allowed to stand in the 

 ice box until the separation was complete when the oily layer 

 was drawn off. This process was repeated. The oil was then 

 treated with a 2 per cent solution of sodium carbonate, washed 

 with distilled water, and dissolved in ether. A small quantity 

 of animal charcoal was added to the ethereal solution; it was 

 then filtered into a 200 cubic centimeter Erlenmeyer flask and 

 evaporated to constant weight on a water bath. It was identi- 

 fied by a determination of its physical and chemical constants. 



Determination of the crude filicin. — The crude filicin was de- 

 termined according to the method employed by Caesar and Lo- 

 retz " which is essentially the same as that given in the Swiss 

 pharmacopoeia. The following is the procedure as carried out by 

 this firm : 



Dissolve 5 grams of the extract in 30 grams of ether, add 100 grams of 

 a saturated solution (3 per cent) of barium hydroxide, and shake the mixture 

 vigorously during several minutes. Transfer to a separator, and run 86 

 grams (4 grams of the extract) of the lower aqueous layer into a flask 

 of 200 cubic centimeters' capacity. Add 2 grams of hydrochloric acid, 

 25 per cent, and shake out with 3 portions of ether, 25, 15, and 10 cubic 

 centimeters. Separate the ether, and filter each portion successively through 

 the same plain double filter into an Erlenmeyer flask of 200 cubic centi- 

 meters' capacity which has been previously weighed. Wash the filter with 

 10 cubic centimeters more ether, and finally distill off the ether and dry 

 the residue at 100° C. Weigh after allowing it to stand in a desiccator 

 for half an hour. The weight multiplied by 25 will g^ive the percentage 

 of crude filicin in the sample. 



'' Jahresb. d. Pharm. (1905), 65, 425. 



