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Monthly record of analytical researches into drugs

 

作者:

 

期刊: Analyst  (RSC Available online 1884)
卷期: Volume 9, issue 12  

页码: 222-225

 

ISSN:0003-2654

 

年代: 1884

 

DOI:10.1039/AN8840900222

 

出版商: RSC

 

数据来源: RSC

 

摘要:

222 THE ANAIjYST. MONTHLY RECORD OF ANALYTICAL RESEARCHES INTO DRUGS. AT arecent meeting of the Pharmaceutical Society, Dr. John C. Thresh made a communication, on the Proximate Constituents of Hedychium Spicatum, of which the following extract embraces the chief points of ohemical interest. Preliminary trials showed that the best solvent of the active principle was petroleum etheie, the extract from this menstruum yielding a crop of crystal which when purified were found t o be tabular, colourless and odourless, soluble in petroleum ether, ether, alcohol, chloroform and benzol. Insoluble in diluted eolutions of potash, soda or ammonia, Sulphuric acid dissolved it in the cold without production of colour, but if heated theTEE ANALYEIT. 223 solution became purple red.The alcoholic solution was neutral in reaction, not coloured by ferric chloride or precipitated by basic lead acetate. It did not reduce silver ealts. Melting point 4900, Mean of two cornbustiona gave C 69*73 per wnt,, H 5.88 per cent., agreeing with formula Ola€€,,O,. By treatment with caustic potash, the cryatah yielded ethyl alcohol, and an acid yielding upon combustion 0 67.63 per cent., and H 5.69 per cent. The silver salt gave 37.55 per cent., metal. The acid therefore had formula C,oH,,O,, and the cq&dline principle CAH3C~oH90d. Upon oxidation with dilute nitric acid, anisic acid was produced in abundance, The acid therefore is methyl paraoxyphenylacrylic, an acid obtained synthetically by Perkin, by the action of acetic anhydride on anisic aldehyde in presence of sodium acetate.The Unorysta;l&~a;bls Portinn of the Petrolmm Bher ResilEzce.-This was found to consist of the odorous principle, a fixed oil and a veryconsiderable proportionof ethylmethylpmcoummte, the latter doubtless prevented from crystallizing by the presence of the former. Upon saponification of the mixture with alcoholic potash, two crysttrtlline acids were obtained, the methylparacoumaric and another, apparently a fatty acid. This latter was totally insoluble in boiling water, but cryatallizable from alcohol. The quaiitity obbined did not enable me to identify it with certainty, and its further exadnation is reserved for the immediate future. The odorous principle evidently exists in the rhizome in very minute proportion, and to isolate it in a state of purity will necessitate working on a much larger quantity of material. A very rninute quantity of the oily fluid above mentioned dropped upon the clothes renders them highIy odorous for a considerable length of time, or if esposed causes a large room to be pervaded with its odour, which to me recalls that of hyacinths.The proximate analysis of the rhizome gave the following results :- Soluble in petroleum ether- Soluble in doohol- Ethylmethyl artwownarrtte , , ~ixed oil md'odorous body . . Indif. substance ppt. by hnnin Acid resin, &c. . . . . Glucoside or sacoharine matter Mucilage.. a , .. *. Albuminoids, orpnic acid, &c. Staroh.. . . . . . . . . adoiaturo . . . . . . . . Ash a 0 * * .. Cellulose, &o... . . . . . . 1 Soluble in water- .. . . . . 3.0 . . . . . . 2*9 1 '" . . . . . . . . 2.7 . . . . . . . . 1.0 . . . . . . . . 2.8 . . . . . . . . 1*9 . . . . . . . . 62.3 . . . . . . . . 13.6 . . . . . . . . 4.6 . . . . . . . . 15.2 10090 - 'the cod-liver oil supplied to the European markets is often spuriow, being either a mixture of the genuine oil with seal or coalfish oil, or else simply the latter oils, alone or mixed, Japan also furnishes the market with so-called cod-liver oil, In order to find, if possible, a test for pure cod-liver oil, A. Eremel has made extensive experiments with oils of known origh. He determined specific gravity,224 THE ANALYST. amount of potash necessary for saponification, and amount of iodine solution necessary for iodizing the oil, but finally came to the concluaion t h t the best process for distinguishing the pure from the spurious oils may be based upon their behaviour with filming nitric acid, spec.gr. 1.500, as follows :- Ten to fifteen drops of the respective oils aze poured on match glasses, and two 01- three drops of fuming nitric acid are slowly run in from the side, when the several oils exhibit the following appearances : 1. Gemline cod-liver oil (from Gadw iliorrha) turns ~ e d at the point of contact ; when afterwards stimed with a glass rod it becomes fiery rose-red, soon passing into pure lemon yellow. 2. Coalfish oil (from Gadus Carbonarius) turns intensely b h e at the point of contact ; when stirred it turns brown, and remains so for two or t h e e hours, when it finally passes likewise into a more or less pure yellow.3. Japanese cod liver oil behaves like the preceding, except that red streaks are some- times observed along with the blue ones, on the addition of nitric acid. All three varieties likewise yield the well-known colour. reaction for biliary acids (with sulphuric aoid). 4. Seal oil, treated as above stated, at first Bhows no change of colour, and becomes brown onIy after some time. As this oil is not a liver oil, it, of course, does not give the reaction for biliary acids. According to the author, this reaction for the spurious oils with fuming nitlic acid is so intense and characteristic, that admixtures of them (of not less than about twenty-five par cent. to genuine oil) may be readily detected. Some time ago, S. G. Bradford recom- mended solution of subacetate of lead as a test for cotton oil in both cod-liver oil and in olive oil, by producing a red colour when the former oil was present.Moreover, a mixture of solution of subacet&e of lead with cod-liver oil causes saponification at omo when shaken in the cold. When cotton-seed or any other oil is present, this saponification will not take place, no matter how long the mixture is allowed to stand, or how well it is shaken. The strength of ether is almost universally judged by the test of specific gravity It is, cousoquently, of great importance that the density of absolute ether should be accurately determined. Authorities differ very much on this point. Various points ranging between 0690 aEd *720 are stated, and though some of the discrepancies may be accounted for by the different temperatures at which the estimations were made, there still lacks uniformity. In an article in the +hemera's, Dr.Squibb discusses the matter, and gives the result of a number of experiments made in order to determine the point. He acknowledges the difficulty in getting ether free from the last traces of alcohol, water, and air, and overcoming the extreme sensitiveness to heat of so volatile a fluid. His conclusions are not, so far, absolutely final, as he promises to continue his investigations when the cold weather shall have fairly set in, but for the present he gives the specific gravity at 4 C. as -73128, and at 1 5 O C. *71888 or *?I890 at 609 F. According to a table of specific gravities of various mixtures of absolute ether and alcohol of Sp. (3. *820, the official ether of the B.P., which is of the Sp. (3. -720, would contain 1 per cent. alcohol, and that of the Sp. G. 735, about 13 per cent. Dr. Squibb does not find the general statement that one volume of ether will dissolve in 10 volumesTHE ANALYST. 225 _ _ _ _ ~ - - of water to be correct. His experiments give one in 11.1 even at a temperature of 2 5 O C. Tho tests foy alcohol in ether he doea not find satisfactory. Admixture with an ecjual volume of copaiba or carbon bisulphide is not sensitive to 01 per cent., while the test with fuchsine is really not a test for alcohol at all, and for water is too sensitive for practical use. Hager’s modification of Lieben’s test is considered the best, but for very accurato dstermhations requires great care, and even then the results are not absolutely certain. In reference to Dr. Squibb’s experiments, it may be noted that absolute ether for anaxthetic purposes is commonly sold in England at a specific gravity of -717 at 60°B.

 

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