Analysis of the Root of Stillingia sylvatica.
By WILLIAM BICHY, PH.G.
Abstract from a Thesis.
Moisture.—Two grams of powdered stillingia root were placed in a weighed porcelain crucible, and dried in a current of air at 110°C. until it ceased to lose weight. Loss, 0.31 Gm., or 15.5 per cent.
Ash.—5 Gm. of the drug were ignited at a low red heat, in a suitable vessel, until all carbon was consumed, yielding 0.25 Gm. of ash, equivalent to 5 per cent., of which 0.051 was soluble in water, 0.101 in hydrochloric acid, 0.027 in sodium hydrate, and 0.071 was insoluble.
Benzol Extract.—20 Gm. of the drug, in No. 80 powder, were moistened, placed in a percolator, and completely exhausted with benzol. The combined percolate measured 150 cc., and yielded 1.0 Gm. of extract, equivalent to 5 per cent. The extract was soft, of a reddish yellow color, and consisted of resin, fixed oil, volatile oil, and coloring matter. Water dissolved 0.15 Gm. of the extract, alcohol 0.55 Gm. (also soluble in ether and carbon disulphide), and 0.3 Gm. was insoluble in water and alcohol. The solution of the extract in water, tested for alkaloids by phosphomolybdic acid, platinic chloride and other reagents gave negative results; and when boiled with HCl, neutralized with KHO, gave negative results with Fehling's solution as a test for glucosides.
Alcohol Extract.—The stillingia treated with benzol was dried at a moderate heat and exhausted with 80 per cent. alcohol; the combined percolate measured 350 cc., and yielded 4.396 Gm. of extract, equivalent to 21.98 per cent. The extract was treated with water, and the tannin estimated with a freshly prepared solution of gelatin and alum. The precipitate weighed 5.16 Gm.; estimating 45 per cent. of this as tannin, a net result of 11.61 per cent. is shown. This tannin produced a green color with iron salts, and white precipitates with solutions of tartar emetic and morphine.
The filtrate recovered from the tannin estimate was acidulated with H2SO4, mixed with an equal volume of alcohol, filtered, evaporated free of all alcohol, and The acid solution tested for alkaloids and glucosides, with results showing the latter to be absent. With phosphomolybdic acid, solution of platinic chloride and Mayer's solution precipitates were obtained. The remaining acid solution was then carefully neutralized with ammonia, and the resulting precipitate treated with 95 per cent. alcohol, which upon evaporation yielded an amorphous powder. After several unsuccessful trials to obtain an additional amount of the alkaloid the following plan was devised: The powdered drug was mixed with one-third of its weight of slaked lime and dried; the mixture was treated with alcohol until exhausted; dilute sulphuric acid was added, the liquid filtered, evaporated free from alcohol, and on neutralizing the acid solution the alkaloid was obtained. When heated it was entirely volatilized; treated with KHO, ammonia evolved; with H2SO4 it combines to form a sulphate, which was obtained in fine scale-like crystals. For this alkaloid I propose the name of Stillingine.
Cold Water Extract.—The drug, after the alcohol treatment, was macerated and percolated with cold water until exhausted; the percolate was of a straw-yellow color, yielded an extract weighing 0.55 Gm:), or 2.75 per cent. It was found to be principally gum. Strong alcohol and solution of subacetate of lead produced copious precipitates.
Acid Extract.—After drying the residue of the foregoing operation it was found to weigh 10.648 Gm. It was mixed with 400 cc. of water and 10 cc. of H2SO4, boiled continually for eight hours, water being occasionally added to preserve the quantity. The liquid now contained all the starch of the root as glucose; it was thrown upon a filter, and thoroughly washed with warm water until the filtrate measured 800 cc. Fehling's solution showed the presence of 4.3243 Gm. of glucose, which was formed from 3.89187 Gm. of starch. The weight of the insoluble portion after drying was 5.902 Gm.; total acid extract, therefore, 4.746 Gm., and of acid extract, not starch, 0.86413 Gm., making the total acid extract 23.73 per cent.
Alkali Extract.—The above remainder was boiled for 3 hours in 200 cc. of a 10 per cent. solution of NaOH, filtered, and washed with water to remove all alkali; the residue after drying weighed 4.592 Gm., making the alkali extract 1.31 Gm. The insoluble residue consisted of crude fibre and ash; to obtain pure cellulose it was macerated for 24 hours in a solution of chlorinated soda, washed, dried, and now weighed 4.367 Gm. This contained 0.355 Gm. of ash, leaving for pure cellulose 4.012 Gm., or 20.06 per cent.
Volatile Principles.—100 Gm. of the finely powdered drug were placed in a retort, macerated for 48 hours with water and distilled; the distillate was neutral, of a straw-yellow color, and possessed a very strong, disagreeable odor. On the surface of this distillate oil was found weighing 3.25 Gm., equivalent to 3.25 per cent. The distillate was tested for alkaloids by the usual tests with negative results.
On summing up the result of the different operations the following is produced:
|Benzol extract (resin, fixed and volatile oil, coloring matter)||5.00|
|Alcoholic extract (tannin., alkaloid, resin)||21.98|
|Aqueous extract (gum)||2.75|
|Acid extract (starch)||23.73|
|Alkali extract (coloring matter)||6.55|