154 



sulphuric acid solution of the alkaloids from 50 grammes of seed 

 was fluorescent, but only so slightly, that error was not completely 

 excluded. Moreover quinidine also fluoresces in sulphuric acid solution. 

 In order to obtain certainty a kilogramme of Ledgeriana seed 

 was powdered and sieved (B 40). In quantities of 20 grm. the powder 

 was mixed with 5 grm. of calcium hydroxide and then 6.5 grm. of 

 5 7o sodium hydroxide and 9.5 grm. of water were added and the 

 mixture v^as stirred for about 2 hours until a suitable granular 

 mass was obtained. This mass was extracted with benzene in a 

 Soxhlet apparatus. 



After distilling off the benzene there remained in the flask, in 

 addition * to the alkaloids and other impurities, so much of an oily 

 liquid that it was impossible to estimate the alkaloids directly in 

 the residue. 



It was found necessary first to free the seed from the oil contained 

 in it before an accurate estimation of the alkaloidal content could 

 be undertaken. 



A preliminary experiment showed that petroleum ether is most 

 suitable for this purpose, since it dissolves the oil, but not the 

 alkaloids. 



The finely pow^dered seed was first completely extracted with 



petroleum ether; the mass was dried, powdered again and sieved. 



Of this powder quantities of 20. gr. were thoroughly mixed with 



slaked lime, caustic soda, and water and the mass was then extracted 



with benzene as described above. 



After extraction and before distilling off the benzene, 10 c.c. 

 of N/^^ hydrochloric acid were added. In this way I finally obtained 

 an almost colourless solution of the hydrochlorides of the alkaloids. 

 After filtering through cottonwool and washing, a drop of a 0.5 "/„ 

 solution of methylred in alcohol was added, the liquid was heated 

 on a waterbath and then titrated back with ^/,, sodium hydroxide. 

 The average result of a few dozen fairly concordant analyses 

 was 0.380 7„ of total alkaloid, calculated for seed containing fat, 

 but no water. These titrated neutral solutions were mixed and 

 evaporated to about 50 c.c, after adding a further small quantity 

 of N/20 sodium hydroxide, so that the liquid was slightly alkaline. 

 After cooling, the liquid was freed from suspended impurities by 

 filtration into a separating funnel. It was then washed, and after it 

 had been made strongly alkaline, it was extracted several times 

 with ether. 



The ethereal solution containing all the alkaloid from a kilogramme 

 of seed, was evaporated to dryness, and the residue was dissolved 



