XXIX] DRUGS 359 



Caffein, Acetanilid and Quinin Sulphate in Mixtures. 



21 preparation of sample and solution.-tentative. 



Transfer to a scparatory funnel one or more average unit doses of the powdered 

 sample, add 20 cc. of water and 50 cc. of chloroform, then 10 drops of dilute sulphuric 

 acid and extract in the usual way. After clearing, wash the solvent in a second 

 separatory funnel with 5 cc. of water prior to transferring to a 200 cc. Erlenmeyer 

 flask. Repeat the foregoing operations with two 50 cc. portions of chloroform, 

 finally distilling the combined chloroform solution to about 10 cc. by gentle heat. 



22 CAFFEIN AND ACETANILID.— TENTATIVE. 



Treat the chloroform residue obtained in 21 as directed under 3 and 4. 



23 QUININ SULPHATE.— TENTATIVE. 



Combine the wash water, used in the second separatory funnel in 21, with the 

 solution of quinin bisulphate, add a slight excess of solid sodium bicarbonate, ex- 

 tract with three 50 cc. portions of chloroform, wash each portion with 5 cc. of water 

 in a second separatory funnel and then pass through a dry filter into a 200 cc. Erlen- 

 mej^er flask. Distil by gentle heat to about 5 cc, evaporate on a steam bath 

 to apparent dryness, dissolve the amorphous alkaloid in 5 cc. of neutral alcohol 

 and titrate with N/50 hydrochloric acid to a faint red, using 2 drops of methyl red 

 as an indicator. Heat on a steam bath until most of the alcohol has been expelled, 

 adding, if necessary, sufficient acid to maintain the acid reaction. From the total 

 number of cc. of acid employed in the titration calculate the quinin sulphate. One 

 cc. of N/50 hydrochloric acid is equivalent to 8.73 mg. of quinin sulphate. 



If the mixture contains acetphenetidin in place of acetanilid, proceed as out- 

 lined above, except that the separation of caffein and acetphenetidin is conducted 

 as directed under 6 and 7. 



Caffein, Acetanilid and Codein Sulphate in Mixtures. 



24 prspar\tio.v o? s\m?l3 axd sdlunox.-tsxrative. 

 Proceed as directed under 21 . 



25 caffein and acetanilid. -tentative. 

 Proceed as directed under 22. 



26 CODEIN sulphate.— tentative. 



Proceed as directed under 23 to the point indicated by the sentence "Distil by 

 gentle heat to about 5 cc". Transfer the chloroform solution of codein with suffi- 

 cient solvent to a small, tared beaker, evaporate to apparent dryness on a steam 

 bath, add a few drops of alcohol to the amorphous residue, then a like amount of 

 water and evaporate again. Finally cool and allow the usually crystalline product 

 to stand until the weight becomes constant. The weight of this residue multiplied 

 by 1.3144 gives the quantity of codein sulphate present. 



This result should be checked volumctrically. Dissolve the residue in 3-5 cc. of 

 neutral alcohol and titrate with N/50 sulphuric acid to a faint red, using methyl 

 red as an indicator. From the number of cc. of standard acid employed calculate 

 the amoimt of codein sulphate. Ojic cc. of N/50 sulphuric acid is equivalent to 

 7.87 rag. of codein sulphate. The quantity of codein sulphate as found by weight 

 will usually be slightly greater than that determined by titration. 



