NOTES IN PHARMACY, No. 3.

EXTR. LIQ. CUBEBÆ.

The coarsely powdered cubebs, being lightly packed in a displacement funnel, I pour upon it as much of a mixture of equal parts of ether and spirit of wine, as it will imbibe, and, having covered closely the top of the apparatus with moistened bladder, and corked the lower aperture, allow it to stand for twenty-four hours. I then uncork it, and after it has ceased {194} dropping, displace the remainder with Sp. Vin. Rect. until the original quantity (generally a pint,) be obtained; this I set aside in an open and shallow vessel to evaporate spontaneously, until all the ether, and most of the spirit has passed off, reducing the quantity to about one half. I then obtain, by displacement with diluted alcohol, another pint of the liquid, exposing it in the same manner, until three-fourths of the quantity is evaporated spontaneously as before; again another pint is obtained by displacement with water, (this will be a proof spirit tincture,) which is added to the former, and allowed to lose by the same means, about one-fourth, or sufficient to leave a resulting quantity of one and a half pints, which will contain about eight ounces of alcohol. The displacement with water is continued to exhaustion, when enough fluid will be obtained to raise the quantity, when added to that already prepared, to two and a half pints, which is transferred to a proper bottle, and there is dissolved in it sixteen ounces of white sugar, yielding, in toto, three pints of fluid extract, equal to one pound of the berries, one f

i of which represents

j of the dry powder. The dregs, when dried, are destitute of sensible properties, appearing to be merely ligneous remains, and the loss in weight, when time is had, may be easily calculated and compared with the recorded analyses. The extract has the appearance of a somewhat thick, brownish colored liquid, possessing the peculiar taste and smell of the cubebs in a remarkable degree, remaining homogeneous for some time after agitation, and showing after settling a large proportion of the oleaginous constituents of the berry. Having aimed more at efficiency than beauty in this preparation, I claim for it the former rather than the latter, and if it should not invite the eye, it will be found very agreeable to the palate. Fluid extract of valerian may be prepared by the same process, and, indeed, all those of a volatile nature, whose active principles are soluble in any of the above menstrua.

UNG. AQUÆ ROSÆ.

UNG. PERUVIAN.

PHARMACEUTICAL ETHICS.

Various are the unworthy practices, one or two of which are thus curtly alluded to, deserving of a more studied notice and severe censure, than I am able or willing to give them. Such matters, though not exactly “putting money in the purse,” should be attended to. The purging of our profession—for it is one—of them, would be a highly meritorious service.

CHLORIC ETHER. BY J. F. HOLTON, PROFESSOR OF BOTANY IN THE NEW YORK COLLEGE OF PHARMACY.

In the early part of this century, some chemists in Holland found a peculiar oily fluid of very fragrant smell, resulted from the action of chlorine on Olefiant gas. It is generally known as the Dutch liquid; it has been called also chloric ether and bichloric ether. Its composition is C4 H2 O2.

In 1831, Mr. Samuel Guthrie of Sackets Harbor, in this State, distilled alcohol from the so called chloride of lime, and obtained a product so closely resembling the Dutch liquid that he though it identical. From some relations to formic acid, it was afterwards called Chloroform, and chloroformid. Its composition is C4 HO3. In 1847, anaésthetic properties brought {198} chloroform prominently before the public. We find an article by Prof. B. Silliman, Jr., in the American Journal of Science, new series, vol., 5, p. 240, in which it is stated that “the terms chloric ether, bichloric ether, perchloride of formyle, Dutch oil and oil of Dutch chemists, are all synonyms of chloroform.”

In a recent visit of the writer at New Haven he saw a prescription of “chloric ether.” Being reminded of the singular error in the Journal printed there, he inquired into the nature of the article dispensed. It proved to be a solution of chloroform in alcohol, and on his return to this city he found the same practice here to a small extent. The proportions in the article bearing this name vary greatly; often it seems that the mere contents of the wash-bottle are in this way disposed of, containing of course a large proportion of water. Mr. Currie, one of our most careful and consciencious chemists, usually prepares it so as to contain 10 per cent. in bulk of chloroform. A more convenient formula would be, chloroform 1 part, alcohol 10 parts. Some such article under the name of Tinctura Chloroformi ought to have place in our pharmacopœia.

But to our confusion the term chloric ether is applied to yet another, and entirely a different body, formed by the distillation of alcohol and hydrochloric acid, the composition of which is C4 H5 O. This is also called hydrochloric ether and muriatic ether.

But to neither of these four substances does the name chloric ether properly belong. Were there such a thing, it would be obtained from the action of chloric acid on alcohol, a reaction which is prevented by the decomposition of the chloric acid by the alcohol, to which it gives part of its oxygen, forming acetic acid.

This subject is not of so much importance intrinsically as it is by way of illustrating the extreme importance of rigid adhesion to systematic nomenclature as the only means of saving us from dangerous errors and inextricable confusion.

{199}

ON THE PREPARATION OF PURE MAGNESIA. BY HENRY WURTZ, M. A.

The preparation of few substances presents such difficulties as that of Pure Magnesia.

It seems, however, at first glance, that the cheapness and general purity of the sulphate which occurs in commerce, would render this an easy task. Unfortunately, however, no simple process has yet been proposed for obtaining pure magnesia from the sulphate. The usual course is to precipitate from the boiling solution with carbonate of soda, and to expel the carbonic acid from the magnesia alba thus obtained, by ignition. On trying this process, however, it was found that the carbonate of magnesia thus precipitated could not be freed from soda by washing. After an enormous quantity of hot distilled water had passed through it on the filter, the slight residue left by evaporation of the washings, still gave the soda tinge to flame.

It is true that the trace of the soda compound thus retained might probably be washed out of the magnesia after its ignition, but the difficulty and tedium of the operation of washing the very voluminous precipitate, together with the expense attendant upon the necessity of using pure carbonate of soda, to avoid the presence of silica, phosphoric acid, and other impurities, which, if present, would inevitably contaminate the magnesia, induced me to reject this method. In fact this method, which was formerly almost used universally by analysts for the determination of magnesia is now rejected by them, except in some unavoidable cases.[16]

[16] H. Ross’s Handbuch, last edition, 2, 33.

The substitution of carbonate of ammonia for carbonate of soda is inadmissible with any regard to economy, on account of the existence of the soluble double sulphates of ammonia and magnesia. A trial was made to decompose sulphate of magnesia by mixing its anhydrous powder with a large quantity of carbonate of ammonia, and igniting, but the only trace of {200} decomposition which appeared was a slight alkaline re-action of the aqueous solution of the mass.

I must here mention an impurity which I have met with in commercial sulphate of magnesia, and this is a double sulphate of magnesia and potash, which occurs in small crystals, apparently rhombohedrons, among the rectangular prisms of the Epsom salt. It may probably be separable by re­crys­tal­li­za­tion, though this, with sulphate of magnesia, is rather a difficult affair.

The method which I adopted for preparing pure magnesia was the ignition of the nitrate prepared from the commercial magnesia alba. The impurities in the commercial carbonate which I made use of were sulphate and chloride, a surprisingly large quantity of silica, a trace of phosphoric acid easily detectable by molybdate of ammonia, oxide of iron, alumina, lime, alkalies and some organic matter. A small excess of this impure article was added to commercial nitric acid and the whole boiled; the silica, oxide of iron, alumina and phosphoric acid were thus separated by the excess of magnesia and the filtered solution contained no trace of either of them; the solution was slightly colored by organic matter.

Either of two methods may now be adopted for separating the lime.

One is to add a late excess of ammonia, then a little oxalic acid, and filter. To this method, besides the expense of so large a quantity of pure ammonia the necessity of the subsequent decomposition and expulsion by heat of the very large quantity of nitrate of ammonia formed is a serious objection.

Unsuccessful attempts were made to separate the lime by adding oxalic acid immediately to the neutral solution of nitrate of magnesia. It was found upon experiment that oxalate of lime is somewhat soluble in a solution of nitrate of magnesia.

The other method, which is preferable, consists in adding to the solution a little sulphate of magnesia, and then a quantity of alcohol, but not enough of the latter to produce any immediate precipitation. If a precipitate is formed immediately, {201} water is added, for, singularly enough, it was found that the liquid filtered from this first precipitate still contained lime. In the course of time the sulphate of lime separates in the form of small crystals.

The filtered liquid is now evaporated in porcelain dishes, and the residue transferred to porcelain crucibles, or still better, to platinum dishes, and the nitric acid expelled by a gentle heat. By a slight modification I have succeeded in shortening this operation very much, that is by adding, from time to time, powdered carbonate of ammonia to the mass, and stirring with a glass rod, or a platinum spatula. When no more red gases are evolved the heat is raised to redness for a few minutes. The mass thus obtained requires washing with pure water to separate alkaline salts and some sulphate of magnesia which it still contains.

Magnesia thus prepared was found, by a most rigid qualitative analysis, to be perfectly pure. I am aware, however, that the process is a troublesome one, and it is very much to be desired that some one would present us with a simple and direct process of obtaining pure magnesia from the sulphate.

ON TINCTURE OF IPECACUANHA. BY G. F. LEROY, OF BRUSSELS.

Officinal preparations during reposition or preservation, when placed in situations proper to preserve them from all changes, yet undergo such important modifications, that the pharmaceutist is frequently obliged to reject them as worthless. We are accustomed to consider alcoholic tinctures, by reason of the vehicle used in their preparation, as amongst the most stable of officinal preparations; and therefore very few {202} pharmacologists have observed the changes they undergo. Amongst those whose attention has been drawn to the subject, I may particularly cite: 1st, Baumé, who has remarked that tincture of saffron deposits a substance analagous to amber.—(Elements of Pharmacy, 2d ed. 1789.)

2nd. Guibourt, who presented to the Academy of Medicine at Paris, some observations on the changes in its composition which tincture of iodine undergoes according to the time when it was prepared, (year 1846.)

3rd. Bastick, with the desire of ascertaining the nature of the changes to which alcoholic preparations are subject, placed various tinctures, during several months, in situations similar to those of a pharmacy, that is to say, exposed to a temperature varying from 60° to 80° Fahrenheit, in bottles half filled, and to which air was, from time to time, admitted.

On examining them, some time afterwards, he found that most of them had undergone active fermentation in a greater or less degree, and that the alcohol had gradually become converted into acetic acid. The tinctures had generally lost their color and taste, and contained a precipitate which was partially re-soluble in a proportion of alcohol corresponding to that which had been decomposed.—(Phar­ma­ceu­ti­cal Journal and Transactions, 1848.)

The tinctures prepared with weak alcohol are the most subject to this species of change.

4th. Tincture of kino changes so with time, that it passes from the liquid to the gelatinized state. This change even affords an excellent test when it is suspected that catechu may have been substituted for kino in this preparation.—(Dorvault, Officine, 1850, 3d. ed.)

In general, pharmacologists consider that tinctures only deteriorate by the evaporation of the alcohol used in their preparation, and that this evaporation has the effect of concentrating them too much, and of giving rise to the precipitation of a part of the principles which were held in solution.

I do not entirely concur in this opinion; on the contrary, I {203} believe that, in many cases, the precipitates which are formed in the tinctures, do not arise from the evaporation of a part of the vehicle, but from a modification which takes place in a part of the principles held in solution, and which, becoming less soluble, or even insoluble, are precipitated.

Amongst these precipitates I shall place that which is almost uniformly found in tincture of ipecacuanha.

Druggists generally are aware that this tincture, shortly after its preparation, throws down a deposite of a yellowish white color, very light, and increasing daily; that when separated by filtration a new deposit immediately commences, and recourse must again be had to filtering.

It is only after three or four filterings, at intervals of five or six weeks, that the formation of this deposit can be arrested. In the course of July of this year, I prepared from the Belgian Pharmacopœia, some tincture of ipecacuanha, to be used in the preparation of some syrup of the same.

Desiring to follow the different phases which it presents, and to study, as far as possible, the nature of the precipitate formed in it, (for as yet I believe that no research has been directed to this subject.) I took advantage of the opportunity which this preparation afforded me.

About six weeks after its preparation, this tincture contained a deposit which was yellowish white, tolerably abundant, very light, and rising on being shaken.

I again suffered the precipitate to form, and after some days, I decanted the clear liquor, and threw the deposit on a filter. I afterwards mixed the decanted liquors and that which was filtered, in a bottle.

The precipitate remaining on the filter, I repeatedly washed. I put it to dry spontaneously, but perceiving, after twenty-four hours, that it was becoming the prey of a number of little cryptogami, formed in the same manner as in animal gelatine which dries slowly in the air, I hastened the desication by carrying the filter into a medium of from 30° to 35° centigrade. {204}

This deposit, during the process of drying, loses its hydrogen, changes color, becoming reddish brown, and is slightly translucid, when very dry it is friable.

The quantity obtained in this first filtering, weighed 5 grains of the Netherland weights, or 0,3250 milligrammes; from an ounce or 32 grammes of roots, employed towards the end of October, I again saved the deposit which was formed: it weighed 1 grain, Netherland, or 0,065 milligrammes.

At present, at the end of November, a third deposition is taking place, and will be collected to be added to the others.

During the whole time the tincture had no effect either upon blue or red litmus paper.

Physical properties. The precipitate is solid, friable, of a reddish color, slightly translucent, without taste.

Chemical properties. Ether, alcohol, water, cold or boiling, have no action upon it; dilute hydrochloric, sulphuric and nitric acids, have no action when cold. Concentrated nitric acid, when cold, produces no effect upon it, but if heated to ebullition it attacks it actively, becoming of a brownish red color. Put in a glass tube closed by one only of its extremities, the other being furnished with two pieces of litmus paper, the one becomes blue, the other red. If the tube is placed in the flame of a spirit lamp, in a few instants the matter swells and the reddened paper becomes again blue.

Placed on a slip of platina, and exposed to the flame of a spirit lamp, it swells, giving out a strong odor of burnt animal matter; it burns without flame and leaves a white ash. This ash treated by reagents, has the char­ac­ter­is­tics of lime.

As may be seen by this short exposition, the deposit is by no means a product resulting from the evaporation of a part of the alcohol, which holds in solution the principles that are deposited, but a particular organic matter united to lime, which is formed at the expense of the azotized principle contained in the roots of the ipecac. What is the azotised principle which concurs in the formation of this substance? Certainly it is not one {205} of those which are commonly met with in vegetables, otherwise the phenomenon which is observed in the tincture of ipecac would be observed in the tinctures made with the other roots. Is it the emetine which is decomposed? If that be the case, the tincture of ipecac would be considered rightly an uncertain preparation.

From the character assigned by M. Willigh to his ipecacuan acid, as well as to the tribasic salt of lead, (Journal de Chimie et de Pharmacie, Octobre, 1851,) it will be readily understood, how I at first thought, without, however, having made any serious researches, that it might be this acid united with the lime, to which the precipitate was owing. But the analysis made by that chemist, which denotes the absence of nitrogen in its composition, does not permit us to entertain this idea.

As will readily be perceived, my researches are far from complete, as I had not a sufficient quantity of the precipitate at my disposition. But while waiting to complete them, I did not wish to delay acquainting the learned world with a fact which appears to me extraordinary and until now unique, and at the same time to call to it the attention of those better situated than myself to pursue such researches.—Presse Medicale Belge.