is that its value shall be the same relative value that one obtains in a larger specimen; for instance, 100 cc. of conium seed weighed 52 grams; 500 cc. weighed 259 grams, which is only 1 gram less than 5 × 52. It may, therefore, be taken for granted that the 100 cc. volume is sufficient for conium. From the shape and size of the particular illustration, one would expect in advance that 100 cc. would be ample, but in some instances, such as cloves, experimentation is necessary. One hundred cc. of cloves weighed 35 grams, 200 cc. weighed 75 grams, which is 5 more than twice the weight of 100 cc. The conclusion in that instance is that a 100 cc. sample is not sufficient for the purpose. As another illustration: 100 cc. of juniper berries were found to weigh 32 grams and 200 cc. weighed 64 grams. The conclusion is that a 100 cc. sample is satisfactory.

Attempts to secure certain supplies, such as different samples of Kamala and Lycopodium, have been thus far unsuccessful. C. J. Zufall (U. S. Food and Drug Inspection Station, U. S. Appraiser's Stores, New York, N. Y.) has informed the associate referee that he has collected considerable data, which he will submit later. The work should be continued.

PART III.

Extended experiments were undertaken to establish the usefulness of micro-sublimation in food and drug analysis. The results were quite satisfactory. A critical study of the apparatus recommended in the literature resulted in the development of improved apparatus and methods. The sublimation of santonin from wormseed, and its subsequent identification may be of especial interest. Within recent years, importations of santonin-free wormseed necessitated careful examination of every shipment. No definite microscopical differences of the santonin-free drug from the one containing santonin have as yet been detected. In fact, it is not clear whether the santonin-free drug is collected from a different species, a physiological variety containing no santonin, or collected too late in the season. A simple test showing the presence or absence of santonin in a sample of wormseed is therefore of especial value. While Tunmann, Heyl and Molisch obtained no satisfactory results, the experiments of the associate referee in subliming this drug were quite successful. The details, however, have not been sufficiently tried out by collaborators to warrant the associate referee recommending the adoption of this procedure as a tentative method.

PART IV.

The subject of conditions existing in the interstate and import trade of crude drugs has been discussed to a more or less detailed extent in recent publications of the Bureau of Chemistry, and especially the Pharmacognosy Laboratory'. It may, however, be of interest to demonstrate here some of the drugs which were found to be adulterated in whole or in part by other plant products.

1 J. Am. Pharm. Assoc., 1919, 8: 725, 717, 459.

Such drugs as hydrastis, aletris, sassafras, as well as pennyroyal leaves are more often found dirty, due to improper collection, than adulterated with other drugs. The standards existing for the maximum allowance of ash are evidently not based on the actual ash content of these drugs, but are arbitrarily fixed and are often much in excess of the natural ash content. The high ash, as the great amount of acid insoluble ash indicates, is due largely to sand or other mineral matter adhering to parts of the drug. This adhering sand apparently can not be readily removed other than by washing the drug at the time of collection, especially for root drugs. The surprising fact that no ash standard exists in this country for hydrastis may again be given emphasis1.

With regard to foreign drugs, substitution is far more frequent, and the drug desired may be substituted either wholly or in part. The substitution products are generally closely related to the drug, the name of which is usually adopted in invoicing and labeling, or the substitute may only have superficial similarity. As examples, may be mentioned the substitution of sarsaparilla root by non-official sarsaparilla species, such as Smilax utilis Hemsley, Brassica juncea (L.) Cosson, (Indian mustard), by Brassica napus var. dichotoma Prain, (Indian rape), Arnica montana L., by Heterotheca inuloides Cass., and castor beans by Jatropha curcas L. products derived from plants belonging to the same families. In the case of foreign drugs, identification is far more difficult, if not at times impossible. The greatest difficulty is experienced with tropical or oriental drugs where insufficient data are available in literature, and often no comparative material is available at the museum. The extension and centralization of collections of natural plant products found anywhere in the world, with botanical specimens, is urgently needed.

RECOMMENDATIONS.

It is recommended

(1) That work be continued to determine the value of a more extended use of volume weight determination in the analysis of crude drugs and spices.

(2) That work be continued to find new sources of supplies or proper substitutes for drugs not now available.

(3) That the subject of sublimation for the analysis of plant products, etc., be further studied.

(4) That the methods for the macroscopic and microscopic identification of Digitalis thapsi (Spanish digitalis), a recent substitute for Digitalis purpurea, and Hyoscyamus muticus (Egyptian henbane), a substitute for Hyoscyamus niger, be adopted as tentative methods.

1 J. Am. Pharm. Assoc., 1920, 9: 779.

REPORT ON ALKALOIDS.

By A. R. BLISS, JR. (Emory University, School of Medicine, Emory University, Ga.), Associate Referee.

It is recommended

RECOMMENDATIONS.

(1) That the following be added to the method for the assay for strychnin in tablets1, to follow, "Dry at 100°C. to a constant weight and weigh as strychnin":

Check the weight of the strychnin by dissolving the residue in neutral alcohol, adding an excess of N/10 sulphuric acid, and titrating back with N/50 potassium hydroxid, using methyl red as the indicator. One cc. of N/10 sulphuric acid is equivalent to 0.0334 gram of strychnin and 0.0428 gram of strychnin sulphate. The U. S. P. factor for strychnin to strychnin sulphate is 1.2815.

The entire method should be further studied.

(2) That the following be added to the assay for strychnin in liquids (applicable to elixirs of iron and strychnin in the absence of other alkaloids), to follow, "Dry at 100°C. to a constant weight and weigh as strychnin”:

Check the weight of the strychnin by dissolving the residue in neutral alcohol, adding an excess of N/10 sulphuric acid, and titrating back with N/50 potassium hydroxid, using methyl red as the indicator. One cc. of N/10 sulphuric acid is equivalent to 0.0334 gram of strychnin and 0.0428 gram of strychnin sulphate. The U. S. P. factor for strychnin to strychnin sulphate is 1.2815.

The entire method should be further studied.

Comments.-The experiences of practically all workers in the alkaloidal field have shown rather conclusively the advisability of the volumetric check on the assays for the majority of the alkaloids.

(3) That the following method for the separation of quinin and strychnin be adopted as a tentative method:

Treat 50 mils of the sample in the usual way with citric acid and ammonia water, remove the precipitated alkaloids by shaking with ether-chloroform, and recover the mixed alkaloids by careful evaporation in a tared dish. Note the weight of the mixed alkaloids.

Dissolve the mixed alkaloidal residue in chloroform, add an excess of 5% sulphuric acid, and then entirely boil off the chloroform on a steam bath. Transfer the solution to a separatory funnel, and wash the dish with sufficient water to make a volume of about 250 mils. (One gram of strychnin requires 6420 mils of water for solution3.)

1 J. Assoc. Official Agr. Chemists, 1919, 3: 189; 1920, 3: 379.

2 Ibid., 1920, 3: 379.

U. S. Pharmacopoeia, IX, 1916, 349, 416.

Then extract it with two 15-mil portions of ether, rejecting the ethereal fractions. Add an excess of ammonia water, and shake out the mixture with 7 portions of ether, using 35, 20, 10, 10, 10, 10 and 5 mils, carefully washing the stem of the separatory funnel each time and running such ether used for washing into the combined ethereal fraction. Wash the combined ethereal fraction with 5 mils of water and allow it to stand for 15 minutes to completely separate. Introduce a pledget of absorbent cotton into the stem of the separatory funnel, and very carefully run the ethereal fraction into a tared dish. Pour 5 mils of ether into the separatory funnel and run into the tared dish; repeat with 5 additional mils of ether. Finally, carefully wash the outside of the stem of the separatory funnel with ether, and run this also into the tared dish. Then very carefully evaporate the ethereal solution on a bath at 100°C. for an hour and weigh as quinin.

Shake ut the ammoniacal liquid left after the foregoing treatments with ether with 7 portions of chloroform, using 35, 20, 10, 10, 10, 10 and 5 mils, carefully washing the stem of the separatory funnel with chloroform and running this chloroform also into the combined chloroformic fraction. Wash the combined chloroformic fraction with 10 mils of distilled water, and allow it to stand for 15 minutes. Introduce a pledget of absorbent cotton into the stem of the separatory funnel, and carefully run the chloroformic solution into a tared dish. Add 10 mils of chloroform to the contents of the separatory funnel, thoroughly agitate the mixture, and, when completely separated, run the chloroformic layer into the tared dish. Wash the outer and inner surfaces of the separatory funnel with a little chloroform, and run this also into the tared dish. Lastly, evaporate the chloroformic solution very carefully on a bath, removing the dish from the bath as the last portions evaporate. Dry the residue at 100°C. for 1 hour, and weigh as strychnin.

This method should be further studied.

Comments. Although this method has been submitted to the collaborators, sufficient time has not yet elapsed for reports of individual results, modifications, criticisms, etc. The associate referee's work with this method has been reported'.

Notes. (a) The solution in chloroform with the addition of an excess of sulphuric acid, followed by the complete removal of the chloroform by boiling, is carried out to insure complete solution of the alkaloids.

(b) The extraction with two portions of ether at this point, before the precipitation with ammonia water, is carried out to remove the traces of oily matter derived from the oils usually used in flavoring an elixir.

(c) The volumetric check on the alkaloids is omitted because, in the case of the alkaloid quinin, it is unsatisfactory and gives simply a rough check, and, in the case of the alkaloid strychnin, the amount of the alkaloid usually obtained by gravimetric process from a 50-mil sample of the usual elixir is too small for volumetric check.

(4) That the following methods for the assay of physostigma and its preparations be adopted as tentative methods:

1 J. Am. Pharm. Assoc., 1919, 8: 804.