HARVARD COLLEGE LIBRARY FROM THE LIBRARY OF GODFREY M. HYAMS TRANSFERRED TO CHEMICAL LABORATORY THE AMERICAN JOURNAL OF PHARMACY. JANUARY, 1882. CELASTRUS SCANDENS, LIN. BY C. HENRY BERNHARD, PH.G. From an Inaugural Essay. Nat. Ord. Celastrace. Common Names: Climbing Staff Tree, False Bitter-Sweet, Fevertwig, Staff Vine, Waxwort and Shrubby Bitter-Sweet. In the preliminary examination of this drug I have used, as far as it was found practicable, the method proposed by Henry B. Parsons, Ph.C., in the April number of the "American Journal of Pharmacy,' 1880. I. PREPARATION OF SAMPLE.-The bark was obtained at a wholesale drug house in this city and, after careful garbling, was reduced to a moderately fine powder and placed in a clean dry bottle. II. ESTIMATION OF MOISTURE.-Five grams of the powdered bark were dried for about 4 hours at 200°F., weighing at different times to determine when it ceased to lose weight. Loss, by this treatment, 11.62 per cent. III. ESTIMATION OF ASH.-Two grams of the powdered bark were placed in a weighed crucible and, after careful ignition, the weight of residue was determined. This gave 7.52 per cent. of ash. A. Amount Soluble in Water.-The ash from 5 grams of bark was treated with several portions of distilled water; the amount soluble was 21.92 per cent. The solution was examined and found to contain sulphate, chloride and carbonate of potassium, and sodium. B. Insoluble in Water, Soluble in Dilute Hydrochloric Acid.-The residue from A was treated with dilute hydrochloric acid, which took up 96 per cent. of the remaining ash. The solution contained iron, magnesium, calcium and phosphoric acid. C. Insoluble in Water and in Dilute Hydrochloric Acid, Soluble in Concentrated Sodic Hydrate.-Nearly the entire amount of residue was dissolved and proved to be silica. Jan. 1832. IV. ESTIMATION OF BENZOL EXTRACT.-One hundred grams of the powdered bark were exhausted with pure benzol, and the percolate evaporated until it ceased to lose weight. The amount of extract thus obtained was 8.75 grams or 8.75 per cent., and it was of a yellowishbrown color. This extract was treated with distilled water and with very dilute hydrochloric acid; the solutions examined for alkaloids and glucosides gave negative results. 93 per cent. alcohol took 93 per cent. alcohol took up 5'6 per cent. of the extract. Upon evaporation, there remained a resinous body having a yellowish-brown color and the odor of the drug. An alcoholic solution of this extract gave a precipitate with an alcoholic solution of acetate of lead. The precipitate was collected, washed with alcohol and freed from lead by HS. Upon evaporation there remained a brown amorphous mass, soluble in ammonic hydrate with the production of a deeper color. From this solution it was precipitated by an acid, showing it to be an acid resin insoluble in water. Its alcoholic solution, with ferric chloride, gave a deep greenbrown coloration. An infusion of the bark did not precipitate gelatin from its solution, which would indicate the absence of tannin. The filtrate from the lead precipitate was then treated with an alcoholic solution of sub-acetate of lead, which caused a precipitate; after washing and freeing this precipitate from lead, the alcoholic solution was evaporated, leaving a red-brownish-yellow, amorphous and tenacious mass, sparingly soluble in water. Its alcoholic solution, with ferric chloride, gives a green color due to the acid resin not precipitated by the neutral acetate of lead. The resin in solution, not precipitated by neutral or oxy- acetate of lead, was freed from lead and evaporated, which left a soft, brownishyellow mass having the odor of the drug and, at first, a bland taste, but soon became quite acrid. It is soluble in alcohol, ether, benzol, chloroform, carbon disulphide and sparingly in distilled water. This is a neutral resin. The soft, resinous matter which remains undissolved after treatment of benzol extract with alcohol, as above, is of a greenish-brown color, inodorous, soluble in chloroform, bisulphide of carbon and partly in ether. The substance which remains after treatment with ether is a caoutchouc-like body, very tenacious and elastic, not affected by strong acids or alkalies, is soluble in bisulphide of carbon and chloroform. V. EXAMINATION OF ALCHOLIC EXTRACT.--The powder not dis Jan., 1882. solved by benzol was dried and completely exhausted by 80 per cent. alcohol; the extract thus obtained, after evaporation, was of a soft consistence and of a dark brownish-yellow color, and of a sweet nau seous taste. A. Absolute alcohol took up the greater portion of the alcoholic extract. a. Soluble in Water.-The absolute alcohol extract wat then treated with distilled water which took up a portion. The solution was of a light brown color and reduced Fehling's solution; presence of glucose. Solution of gelatin was not precipitated and no change with iron solution; absence of tannin. Subacetate of lead gave a precipitate, the filtrate containing glucose. b. Insoluble in Water.-b'. Soluble in Dilute Hydrochloric Acid.The absolute alcoholic extract which was insoluble in water was treated with very dilute hydrochloric acid; the resulting solution gave a slight yellow precipitate with Mayer's solution and, upon evaporation, left a slight residue. b2. Soluble in Dilute Ammonic Hydrate.-Ammonic hydrate dissolved the entire amount of extract not soluble in HCl, and it was again precipitated by an acid; acid resin. B. Insoluble in Absolute Alcohol. c. Soluble in Water. c'. Precipitated by Subacetate of Lead.-That portion of 80 per cent. alcoholic extract which was not dissolved by absolute alcohol was treated with distilled water and the resulting solution precipitated with subacetate of lead; the precipitate collected, washed and freed from lead gave, upon evaporation, a brown residue. c. Not Precipitated by Subacetate of Lead.-The filtrate from c1 was freed from lead. Iodohydrargyrate of potassium gave a yellowish precipitate; iodine and iodide of potassium solution, a brown precipitate; phosphomolybdic acid, a greenish-white precipitate, and the same reagent added to an alkaline solution, a blue evanescent coloration. Fehling's solution gave a copious precipitate. d. Insoluble in Water.--d'. Soluble in Dilute Hydrochloric Acid.— The solution gave reaction for glucose. d. The portion insoluble in dilute hydrochloric acid was soluble in ammonic hydrate and reprecipitated by an acid. VI. COLD WATER EXTRACT.-The powder exhausted by 80 per cent. alcohol was next treated with cold water, the infusion concentrated and the gum precipitated with stronger alcohol. This was of a Jan., 1882. fawn color. The alcoholic filtrate still held in solution coloring matter and extractive matters. VII. TREATMENT WITH ACID.-The powder exhausted by cold water was boiled with a 1 per cent. solution of sulphuric acid for six hours, adding water from time to time to preserve the measure. This treatment converted starch and its isomers into glucose. The solution thus obtained was freed from its acid by barium carbonate, and then examined. With Fehling's solution it produced a large amount of precipitate-starch; the aqueous decoction of the bark showed presence of sugar by Fehling's solution, and starch by iodine. VIII. Caustic soda (20 grams to the liter of water) yielded with the powder a brownish-red liquid which was not further examined. The residue now consisted of cellulose. By distillation with water, the bark yielded a volatile oil of a rather agreeable odor. Since, in the above examination, reactions indicative of an alkaloid were obtained, its isolation was attempted from two pounds of the drug by various methods, but without success, and the reactions were therefore most likely produced by other organic matters. The alcoholic tincture contained an acid resin which, after precipitation by lead acetate and isolation, was amorphous, brown or greenish-brown, brittle, inodorous, soluble in ammonia, producing a deep-colored solution from which it was precipitated by an acid; with ferric chloride, its alcoholic solution gave a green coloration; barium hydrate solution added to its ammonia solution produces a brown precipitate. The filtrate from the lead precipitate yielded a red-brownish-yellow mass having the odor of the drug, at first of a bland taste but soon quite acrid. It is sparingly soluble in distilled water; soluble in ether, benzol, chloroform and carbon bisulphide; insoluble in ammonia. RECAPITULATION.-The bark of Celastrus scandens may be said to contain: Acids in combination-sulphuric, hydrochloric, phosphoric and silicic; bases in combination-potassium, sodium, magnesium, calcium and iron; an acid resin and a neutral resin, starch, sugar (glucose), gum, a caoutchouc-like body, coloring matter, extractives and a volatile oil. A tincture of the bark made with dilute alcohol is unstable, producing a precipitate partly soluble in ammonia and partly in alcohol. Glycerin will not prevent this deposit: and, as it is more than probable that the activity of the drug is due to the resins and volatile oil, a |