each bottle covered with a skin of precipitate, and interspersed with little warty resinous-looking concretions. There was a heavy precipitate, greenish-brown in each.

Experiment No. 8, May 14th, 1881.-Fifty pounds of yellow dock root (rumex crispus) were percolated with a mixture of alcohol three parts, water two parts. The percolate was reserved as in experiment No. 1. The second reserve was from the thirtieth pint.

In two hours there was a decided precipitate in the mixture. In twenty-four hours there was a precipitate in all, heaviest in the first percolate. The color of these precipitates was of a dirty yellow. July 7th, there was a precipitate of three-sixteenths of an inch in thickness in the first percolate. This precipitate was dark yellow, but interspersed with bright yellow minute crystalline tufts. The mixture contained about half as much sediment as the first percolate, and the second percolate contained about half that of the mixture. These precipitates are evidently chrysophanic acid more or less impure.

Experiment No. 9, May 21st, 1881.-Eighty pounds of cinchona compound mixture was percolated with a mixture of alcohol three parts, water two parts. The percolate was reserved as in experiment No. 1.

In twenty-four hours there was a precipitate in the mixture. July 7th, there was a precipitate in all, heaviest in the mixture, lightest in the second percolate.

Experiment No. 10, May 21st, 1881.-Eighty pounds of eupatorium purpureum were percolated with a mixture of alcohol three parts, water two parts. The percolate was reserved as in experiment No. 1. In two days they all contained deposits of yellow needle-like crys tals, heaviest in second experiment and in the mixture. These crystals continued to grow until, at the time this is written (July 7th), they fill about one-fourth of each bottle. They are in the form of acicular needles, crystallizing in radiating tufts, some measuring half an inch in length. They are heaviest and in greatest amount in the first percolate.

Experiment No. 11, May 21st, 1881.-Eighty pounds of taraxacum were percolated with a mixture of alcohol three parts, water two parts. The percolate was reserved as in experiment No. 1.

In twenty-four hours there was a yellowish-white precipitate in the mixture and the first percolate. July 7th, there was a precipitate in the first percolate of one-fourth of an inch in depth, composed of a light-colored lower stratum and an orange-colored upper stratum. The mixture contains a thin precipitate, divided, like that of the first percolate, into a light-colored lower stratum and an orange-colored

upper stratum. The second percolate contains a crystalline aggregation over the bottom of the bottle, and this is perfectly white.

Experiment No. 12, May 21st, 1881.-Forty pounds of logwood were percolated with dilute alcohol. The percolate was reserved as in experiment No. 1. The second reserve was taken from the twenty-fifth pint of percolate.

After thirty days there had been no change. July 7th showed a slight yellow precipitate in the mixture.

In commenting upon the aforementioned experiments, I will say that the powders were thoroughly dried. The result supports my theoretical explanation of the formation of a line of precipitates by simply mixing a percolate, and without calling upon chemical action, oxidation, etc. I can say that many other experiments instituted in like manner gave similar results. Arguing, then, simply from the theory of our system of percolation, and comparing it with the evidence afforded by experience and experiments, I must say that it does not seem probable that we shall ever, by percolation alone, succeed in making a line of permanent fluid extracts from dry plants. The most important of steps, then, is to adapt our menstruum so that it may hold in solution the medicinal principles of each plant, and thus render the precipitate which forms inert; for the precipitate will follow. Inasmuch as our coming Pharmacopoeia embraces a line of fluid extracts made by percolation, and as percolation alone cannot produce permanent liquids (if there be any exceptions I have not found them), let us not criticise the committee if, as is to be expected, precipitates continue to form in officinal fluid extracts. It will be noticed that the evidence I bring forward here in the way of experiments is mainly circumstantial, but it is of such a nature as to be almost conclusive. Those that care to follow the idea will find it supported by experiments upon the nature of the precipitates. It is scarcely necessary for me to consume further time upon this point, and I cannot lengthen this paper by the introduction of another subject without making it tiresome.

ON FLUID EXTRACT OF JABORANDI AND ON THE PREPARATION OF PILOCARPINA.*

BY GEORGE W. KENNEDY.

QUERY No. 22.-Jaborandi. Determine the best method for making a fluid extract and for extracting its active principle (pilocarpina).

DURING the past few years a number of articles have been written on this subject, making their appearance in pharmaceutical literature,

*Read at the Third Session.

giving different processes for preparing the fluid extract and also the alkaloid pilocarpina.

In reference to the fluid extract I find writers disagree very considerably as to the best menstruum which should be used. One writer recommends a menstruum composed of one-third alcohol and twothirds water; another favors a menstruum containing fifty per cent. of alcohol; and another claims a menstruum containing not less than eighty-four per cent. of alcohol to be the best.

In devising a formula it is absolutely necessary to take into consideration the active constituents of the drug, if they have been isolated, and their solubilities; then you can proceed intelligently to formulate a process which, when completed, will hold all the active constituents of the drug in perfect solution.

The question may then be asked: What are the desirable constituents of jaborandi which should be present in the fluid extract or any other preparation of the drug? According to good and reliable authority we have a volatile oil, an acrid resin, and pilocarpina. The first two are not of so much importance as the last named. Both Hardy and Gerrard believe they have discovered a second alkaloid, of which, at this time, very little is known.

The volatile oil, as examined by Hardy, who obtained about half of one per cent. from jaborandi, was found to consist of three distinct hydrocarbons, one of which he named pilocarpene, besides an oxygenated oil. The true therapeutic properties of the acrid resin have not fully been determined; it is insoluble in water and soluble in alcohol. Pilocarpina, the principal constituent of the drug, and to which special attention should be given in preparing any of the preparations, has been found to be sparingly soluble in water, but to dissolve freely in alcohol, ether, and chloroform. Knowing then the best solvents for the drug, there can be no difficulty in constructing a formula.

In making the various preparations of the drug, particular attention should be directed to the quality of the drug used. The stems should be rejected, as they have been found to contain little if any of the alkaloid pilocarpina. Some of the specimens, as found in the mar ket, contain a great deal of inert drug, the leaflets being of a brownishyellow color, which are unfit for use, and should be cast to one side. Those only should be selected having a uniform dark-green color, which will be found to possess the full virtues of the drug. If they are purchased indiscriminately and converted into manufactured preparations one can readily understand why one man's fluid extract is much stronger or superior to that of another.

Then again, according to Budee, the leaves of piper lætum appear in the market as Brazilian jaborandi, and in those he failed to demonstrate the presence of an alkaloid.

There are a number of other South American plants sent into the market and sold as jaborandi simply because they have some resemblance to the true variety and possess diaphoretic properties, and these may or may not be inferior to the pilocarpus pennatifolius.

In making preparations of the drug, no matter for what purpose, either as an experiment or for medicinal use, only the leaflets of pilocarpus pennatifolius should be used in order to give proper credit to the drug.

In constructing a formula for the fluid extract, bearing in mind that the active constituents are sparingly soluble in water, freely so. in alcohol, ether, and chloroform, I would recommend the following, which in the hands of the writer has proved satisfactory both pharmaceutically and medicinally:

Fluid Extract.-Take of pilocarpus, in fine powder, sixteen troy oances; alcohol (75 per cent.), sufficient quantity. Moisten the pow der with eight fluid ounces of the menstruum and carefully pack in a conical glass percolator; cover the surface of the moistened powder with a disk of paper, and pour upon it eight fluid ounces of the above menstruum; watch the lower orifice of the percolator and, when the liquid commences to pass, close it with a cork and cover the top with a lid, which should fit closely to prevent evaporation, and permit it to remain in this condition for four days; the cork should then be removed and percolation permitted to proceed slowly,-not faster than forty (40) drops per minute. The above menstruum should be used from time to time as required. Reserve the first fourteen fluid ounces which pass, and continue percolation until the drug is thoroughly exhausted; evaporate to two fluid ounces, and mix with the reserved portion when the extract is completed.

Pilocarpina, or Pilocarpia, as it is called by some writers, at first was named jaborandina, but since the name had already been appropriated, it is now called pilocarpina.

Quite a number of processes have been given for the extraction of this alkaloid, each author claiming for his process advantages over the other, either by furnishing a larger yield or a less difficult process. of manipulation. I would recommend the following process, claiming it to be less expensive and less troublesome:

Take of true jaborandi leaves (pilocarpus pennatifolius) and reduce to a fine powder; moisten the drug with water acidulated with muriatic acid in the proportion of a pint of the former to one fluid drachm of the latter; pack in a glass conical percolator and pour on a sufficient quantity of the above menstruum till it commences to drop from the percolator; close the lower orifice with a cork, and cover the top to exclude air, and allow it to remain in this condition forty-eight hours; afterwards remove the cork and continue percolation with the

same menstruum until two pints are obtained for every pound of drug used; transfer to an evaporating-dish and, by means of a water-bath, evaporate to the consistence of a soft extract; add a sufficient quantity of warm water, enough to permit of filtration; then filter, and treat the filtrate with sodium bicarbonate in slight excess, which is known when effervescence ceases. The object of the soda salt is to decompose the chloride of pilocarpina; the result is liberation of carbonic acid gas, chloride of sodium, and pilocarpina. Then, with a large quantity of chloroform, using one ounce for every ounce of filtered extract, agitate occasionally for ten hours; allow it to subside; pour off the chloroformic solution and evaporate spontaneously; redissolve in chloroform, and evaporate as before. Pure pilocarpina is left, and, as thus obtained, is a soft, glutinous mass; is non-crystallizing, but produces crystalline salts. Its salts, with the organic acids, are uncrystallizable, according to Dr. Squibb.

With iodine, a heavy reddish-brown precipitate is produced.
Tincture of iron, no change.

Salycilic acid, no change.

Bichromate of potash, light blue color; by the addition of sulphuric acid, color is destroyed.

Chloride solution of gold, a heavy lemon-yellow colored precipitate.

ON POWDERED EXTRACTS.*

BY C. S. HALLBERG, CHICAGO.

QUERY 32. Powdered extracts present some advantages at the dispensing-counter. What solid extracts may advantageously be kept in that form, and how are they best prepared?

THE powdered extracts as found in the market are not very satis factory, the slight exposure which they receive during dispensing being sufficient to, in a short time, render them in a hard mass more difficult to manipulate than the ordinary solid extracts.

The writer, after a number of experiments, concludes that this is due to the small percentage of admixture used.

Although powdered extracts are made containing respectively 10 per cent. of admixture, sufficient of inert matter to replace the moisture lost, and such proportion of diluent as to make the extract represent a certain proportion of the drug, these apparently varied amounts will not exceed 10 per cent. of the foreign substance.

Read at the Fifth Session.