THE AMERICAN

JOURNAL OF PHARMACY

APRIL, 1899.

SYRUPUS ALTHÆÆ,

BY F. W. HAUSSMANN,

Research Committee E, Pharmacopœia Revision.

The desirability of a formula for this syrup, which would furnish a preparation possessing greater stability, has been expressed by American as well as Continental pharmacists,

To the former the present official cold process is extremely unsatisfactory, and almost every step in the course of preparation has been subjected to criticism.

Prominent objections, as pointed out by different writers, are the short time directed for macerating the root, the neglect of making allowance for the amount of menstruum absorbed by the althæa and consequent failure of dissolving all the sugar in the strained liquid.

By far the greatest difficulty which confronts the pharmacist, lies however, in the instability of the syrup.

The Pharmacopoeia of 1880 directs recent preparation which, if the time necessary for completion is considered, is impracticable.

The present Pharmacopoeia omits directions for recent preparation, but recommends the syrup to be kept in filled bottles in a cool place.

To secure greater stability the addition of 10 per cent. by volume of glycerin is ordered.

It is, nevertheless a fact, that in warm weather the syrup will rapidly decompose, and in not a few instances fermentation takes place before the syrup is even completed.

Stability of a pharmaceutical preparation in the hands of the con

sumer is equal in importance to its keeping qualities in the shop bottle of the dispenser.

On standing a short time the cloudy syrup will be found to contain a mucilaginous deposit, which appears to be the direct medium of inducing fermentation.

To insure greater stability of the syrup, the whole or a part of the mucilage must therefore be removed.

This would, however, involve the question if the mucilage is of such signal importance, that its presence is absolutely necessary to the therapeutical value of the syrup.

Experiments conducted by the writer and extending over two years, show that a stable preparation can only be produced by removal of the mucilage.

Addition of glycerin is practically valueless as long as cold preparation with presence of the mucilage is directed.

The German Pharmacopoeia, like the U.S.P., directs cold infusion of the althæa in a weak alcoholic menstruum.

The addition of alcohol is necessary to lessen the liability of fermentation in the infusion in warm weather.

The time of maceration should also be increased from one to three hours.

Up to solution of the sugar in the infusion, the working formulas of the United States and German Pharmacopoeias coincide.

The former at this point directs the sugar to be dissolved by agitation without heat, while the latter directs the syrup to be heated to the boiling-point with filtration of the syrup, thus removing a part of the mucilaginous principles.

That this formula is not satisfactory to German pharmacists is demonstrated by the suggestions for improvement occasionally published. Most authors recommend clarification of the mucilage, preparation of the syrup by means of heat, and removal of the scum from the boiling syrup.

Prominent among these modifications is a process recommended by Gesche, published in the Proceedings of the A. Ph. A. of 1895. This consists in preparing the infusion by the cold process, and evaporating the same to definite volume.

Alcohol is now added to precipitate the mucilage, the mixture filtered, made up to a certain volume with water, and the sugar dissolved by heat.

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, 1899

For practical purposes this method is too tedious, and may be modified without resorting to evaporation.

Dieterich clarifies the infusion by means of paper pulp, dissolves the sugar in the liquid by means of heat, and removes the scum from the boiling syrup.

This formula, as published has the disadvantage of not directing a definite weight or volume of the finished syrup.

After a number of trials the following formula was found to furnish a syrup which will not ferment, and possesses the flavor of the althæa.

Specimens, prepared over a year ago, and exposed to all temperature conditions, have retained their original appearance, flavor and consistence.

Wash the althæa with cold water, then macerate it with 400 c.c. of water, previously mixed with the alcohol during three hours, stirring frequently and strain without expression.

Heat the infusion to boiling, add 10 grammes of purified talcum, and filter while hot, passing a sufficient quantity of boiling water through the filter to measure 400 c.c.

Add the sugar to the filtrate, heat to boiling, remove the scum and strain. When cold add a sufficient quantity of water to make the syrup measure 1,000 c.c.

Keep the syrup in completely filled bottles, in a cool place.

Of the several methods experimented with, none furnished as satisfactory a preparation as the one above.

Filtration of the hot infusion without talcum yields a cloudy filtrate, and consequently an inferior syrup, liable to ferment.

Precipitated calcium phosphate, employed in place of talcum, is also unsatisfactory, as larger quantities are required, and a somewhat cloudy filtrate results.

Should it be found necessary for the Pharmacopoeia to retain the present formula, the syrup, prepared by the above process, will be found a decidedly more satisfactory preparation for counter sale.

SYRUPUS ACACIÆ.

By F. W. HAUSSMANN,

Research Committee E., Pharmacopoeia Revision.

This syrup possesses the disadvantage common to all preparations combining saccharine with mucilaginous principles, of turning sour on standing.

Many pharmacists, therefore, prefer to prepare it extemporaneously, and a formula, which can be manipulated so as to furnish the syrup in reasonably short time is desirable.

Some Continental pharmacopoeias have dropped syrup of acacia altogether, leaving it to the judgment of the dispenser to select the method of preparation when ordered.

To American pharmacists the present official process is unsatisfactory.

Besides the time required for the preparation of the mucilage, it furnishes the anomaly of preparing an unstable preparation from another equally liable to decomposition.

Pharmacists who are compelled to keep the syrup on hand, prefer the formula of the Pharmacopoeia of 1870, which consists in dissolving the sugar in a previously prepared mucilage by means of heat.

Others resort to the shortest of all methods, that of rubbing the powdered gum with syrup.

Due to the avoidance of heat, the present official syrup possesses the advantage of being transparent.

No formula for rapid preparation can, however, be based upon the official process, as preparation of the mucilage requires too much time for practical purposes. Syrup of acacia cannot be expected to keep indefinitely.

A formula is therefore required which does not lay claim to staoility as much as ready manipulation.

The writer made extensive experiments with powdered acacia, with the object of elaborating, if possible, an easily manipulated formula. Objections to the use of powdered gum are the impossibility of obtaining a clear preparation and the development of a disagreeable musty odor on standing.

The latter was noticed in every syrup prepared from powdered gum, and its use was therefore abandoned.

Granulated gum was substituted, with better results.

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The point to be observed is to procure an article of good quality, as the color of the finished syrup is influenced thereby. The following formula can be quickly manipulated and furnishes a syrup equal to that of the 1870 Pharmacopoeia. When first prepared, it is somewhat cloudy, soon becoming clear, but does not possess the brilliant transparency of the official syrup.

Mix the sugar with the acacia and add to the distilled water, previously warmed in a capsule.

Stir until dissolved, continuing a gentle heat. Finally add a sufficient quantity of syrup to make the syrup measure 100 c.c.

THE ESTIMATION OF NITRATES AND AMMONIA IN WATER.

BY FRANK X. MOERK.

Read at the Pharmaceutical Meeting of the Philadelphia College of Pharmacy, March 21, 1899.

The quantities of chemicals which have to be determined in water analyses are, as a rule, so minute, that the employment of the usual methods of quantitative analysis means the evaporation of large quantities of the samples to obtain suitable quantities of residue, hence, it is not surprising that within recent years delicate colorimetric tests have largely been made use of, particularly in the estimations of the heavier metals and of the nitrogen-containing compounds like the nitrites, nitrates and the free and albuminoid ammonia.

ESTIMATION OF NITROGEN AS NITRATES.

The method generally used, depends upon the formation of aromatic nitro-derivatives, which have intense coloring power, especially in alkaline solutions; the manipulation used by the writer for some years is as follows: 10 c.c. of the sample are evaporated to dryness in a small porcelain capsule on a water-bath; the residue is thoroughly mixed with I c.c. phenol sulphonic acid (made by