, Jour.Pharm

, 1906

tains much of the information on newer medicaments, which is scattered through the medical journals, but which has not been incorporated in the textbooks. The price of the book is $1.50.

THE ANNUAL LABORATORY REPORT of the Smith, Kline & French Company has been recently published. It contains reports of analyses, besides some original papers. Reports of this kind ought to be in the hands of retail pharmacists, as they show the necessity for testing goods purchased.

PROCTER MONUMENT FUND. The following additional subscriptions have been received :

PROGRESS IN ALKALOIDAL CHEMISTRY, during the year 1904, by Dr. H. M. Gordin, is the title of Monograph No. 10 of the Pharmaceutical Popular Science Series, edited by Dr. Edward Kremers. The articles forming the basis of this monograph have appeared in the Pharmaceutical Review. It is fortunate for the student of pharmacy that these articles have been brought together in this form, as the literature is a rather large and wide one, and the abstracts are unusually full and present a great deal of useful information.

DR. HENRY H. RUSBY is the author of a series of well illustrated and interesting articles on the "Wild Foods of the United States," appearing in Country Life in America. In the September issue there are a number of other interesting articles on trees, fruits, birds, stock, poultry, etc.

HERMAN T. FRITZSCHE, senior member of the firm of Schimmel & Co., Leipzig, died on July 24th, of appendicitis, at Marienbad, Bohemia, where he had gone on account of ill-health.

LLOYD LIBRARY.—It has just been made public that in the will of the late Surgeon-General James Pattison Walker, of England, a clause gives to the Lloyd Library a fund of $30,000, and, what is far more valuable than the cash bequest, the entire library owned by the distinguished surgeon and studentscientist. Gen. Walker's collection of books and manuscripts is known to scientific men as one of the most valuable private collections.

THE AMERICAN

JOURNAL OF PHARMACY

OCTOBER, 1906.

THE ALKALOIDAL ASSAYS OF THE U.S.P. OF 1900.

By H. M. GORDIN.

Having been asked by the editor of this JOURNAL to make a review of the methods adopted in the last edition of the U.S.P. for the assay of alkaloidal drugs and their galenical preparations, I hereby offer a few observations which occurred to me during this examination of the pharmacopoeial methods.

On examining the assay methods of crude drugs it will be noticed that different methods are used for different drugs without any good reason so far as I can see. While it is true that not every method is suitable for every drug, it would nevertheless seem to be advisable to adhere to one and the same method wherever it gives as good results in one case as in another. Comparing, for example, the methods adopted for the assay of aconite, belladonna and ipecac, it is difficult to see why the simple method adopted for the first of these drugs would not give as good and concordant results with the other two. In the same way, on comparing the assay methods for the fluid extracts of cinchona bark, aconite, belladonna and ipecac roots, it would seem that the simple and exact method adopted for the assay of the fluid extract of belladonna root would also give good and concordant results with the other fluid extracts, particularly if ether or a mixture of ether and chloroform were substituted for chloroform. That the methods which give good results with belladonna root and its fluid extract are equally well applicable to aconite root and its fluid extract, for example, is in accord with my own experience as well as with the statements of A. B. Lyons in his well known Hand-book of Practical Assaying of Drugs and Galenicals, where the author uses the same methods for the assay of both of these drugs and their fluid extracts.

In some assay methods of the U.S.P. care has been taken to avoid the use of aliquot parts of the real liquids, while in others no such care is taken.

In some assays solid substances are dissolved in ether or a mixture of ether and chloroform and the solutions transferred to a separating funnel. Thus in the assay of extract of nux vomica we are told to dissolve the extract in an open beaker by means of a mixture of ether, chloroform and ammonia water, and when the extract is dissolved to transfer the solution to a separating funnel. As the extract goes only very slowly in solution, requiring continuous stirring with a glass rod, and the liquid has a great tendency to "creep" on the outside of the beaker when poured into the separating funnel, it is easy to see that much greater accuracy would be obtained by weighing the extract directly into the separating funnel, adding the solvent mixture to the powder and shaking the stoppered funnel till the extract is dissolved.

Some of the assay methods of the pharmacopoeia are completely unworkable. Such, for example, are the assays of aconite root, its fluid extract and fluid extract of ipecac root, in all of which we are directed to filter the first acid liquids obtained in these assays, but as these liquids are very thick and contain sticky resinous substances, the filters are very soon completely clogged and the assays cannot be finished. This is in accord with my own experience and the experience of several teachers and students in our school,

As hydrastis and its galenical preparations are standardized in the new pharmacopoeia an assay method ought also to be adopted for the glycerite of hydrastis.

I shall now take up the individual assays in the order they occur in the U.S.P.

ACONITUM.-AS said before, the assay method is unworkable. Even if it worked it is unnecessarily complicated.1

BELLADONNAE FOLIA ET RADIX. This assay method requires only a few modifications in order to make it simple and exact.

(1) The percolation ought to be continued to exhaustion, as indicated by Wagner's reagent.

(2) The cause of error liable to result from transferring of the creeping" ethereal mixture from one vessel to another and the

See paper read by the author at the meeting of the A.Ph.A., 1906, entitled "Some Alkaloidal Assays." (This JOURNAL, p. 458.)

adhering of drug particles to the sides of the first vessel could be completely eliminated by carrying out the shaking and the percolation in one and the same vessel specially constructed for that purpose.1

(3) As these drugs are rather poor in alkaloid, at least 20 grammes of the leaves or the root ought to be taken for the assay. CINCHONA. Instead of "a mixture of 125 c.c. of ether and 25 c.c. chloroform" the directions ought to be " 150 c.c. of a mixture of 5 volumes of ether and I volume of chloroform previously prepared and cooled to the ordinary temperature." As on mixing ether and chloroform there is a rise in temperature and contraction of volume,' the 100 c.c. drawn off afterwards at ordinary temperature for the assay will from both causes represent more than 10 grammes of drug.

It seems to me that it would be better to use for the assay of cinchona the same method which is used for belladonna root and thus avoid taking an aliquot part of ethereal liquid.

The pharmacopoeia directs to make up the final liquid to 50 c.c. and use half for the estimation of total alkaloids, the other half for that of quinine. It would be more convenient to pipette off 20 c.c. (representing 4 grammes of drug) for each of these estimations. As the drug is quite rich in alkaloids there is no disadvantage in working upon 4 instead of 5 grammes of it.

COCA. The percolation ought to be carried to exhaustion as indicated by Mayer's reagent, and by using the special tube mentioned under belladonna the transferring of ethereal liquid from vessel to vessel could be avoided.

COLCHICI CORMUS ET SEMEN-The use of the shaking-tube would be advisable.

On comparing the methods for the corm and the seeds it will be seen that in the case of the corm the colchicine before it is weighed undergoes an extra purification. If this is desirable in the case of the corm it ought also to be used in the case of the seeds.

CONIUM. The assay method is very complicated and will hardly give concordant results in the hands of different chemists.

EMPLASTRUM BELLADONNAE. It would be preferable to introduce the plaster cut into strips into a separating funnel for the extraction

1 See AMERICAN JOURNAL OF PHARMACY, 1905, p. 463.

2 J. Chem. Soc. Trans., 1897, 371.

with chloroform. When completely extracted the strips could be removed by means of a hooked copper wire.

EXTRACTUM BELLADONNAE FOLIORUM.-It would be preferable to put an indefinite amount of extract into a tared separating funnel and determine the amount of extract taken by weighing the funnel together with the extract.

EXTRACTUM COLCHICI CORMI.-The assay could be simplified by weighing the extract directly into the separating funnel and, after adding ammonia, shaking out the colchicine with chloroform or a mixture of chloroform and ether. The assay could then be finished in the way given in the pharmacopoeia.

EXTRACTUM NUCIS VOMICAE.-Here again the extract ought to be weighed directly into the separating funnel.

Before the removal of the last trace of chloroform from the final residue containing the strychnine a few drops of amyl alcohol ought to be added and the liquid evaporated to dryness by blowing air over the surface of the vessel while the latter is kept on the waterbath. Otherwise there is liable to be loss of alkaloid by decrepitation. As this simple device effectively prevents decrepitation it ought to be adopted.

EXTRACTUM PHYSOSTIGMATIS.-The method is unnecessarily complicated and could easily be replaced by a simpler one.1

EXTRACTUM SCOPOLAE ET E. STRAMONII.-The remarks given under extractum belladonnae foliorum apply also to these extracts. FLUIDEXTRACTUM ACONITI.-As said before, this assay is unworkable. The remarks given under aconite apply also to its fluid

extract.

FLUIDEXTRACTUM BELLADONNAE RADICIS. The method is good and could be made still better by shaking out the first chloroformic solution once or twice more with acidulated water.

FLUIDEXTRACTUM CINCHONAE.-A method similar to the one used for belladonna fluid extract would be preferable.

FLUIDEXTRACTUM COCAE.-The assay method is very good, but could still be improved by shaking out three times with ether instead of twice.

FLUIDEXTRACTUM COLCHICI SEMINIS.-The assay method is very

good.

1 See footnote to aconite.