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Foods and drugs analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1906)
卷期: Volume 31, issue 369  

页码: 404-409

 

ISSN:0003-2654

 

年代: 1906

 

DOI:10.1039/AN9063100404

 

出版商: RSC

 

数据来源: RSC

 

摘要:

404 THE ANALYST. ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. On the Sugar contained in Milk. J. Sebelien. (Festschrift xum 65-j~ihr. Geburtstay von OLaj Hammarsten, No. 17; through Chem. Ztg., 1906, xxx., Rep., 337.)-The author shows that a. pentose, probably arabinose, is present in milk to the extent of about 20 to 40 mgms. per 100 C.C. of milk. Other unknown carbo- hydrates must also be present to explain the differences always found between the gravirnetric and polarimetric determinations made on the milk serum free from proteid, and the different values found when the quantities of Fehling solution used are varied. A. G. L. A Rapid Method of Removing Alcohol from Ether. P. Guigues. (Journ. Pharm. Chinz,., 1906, xxiv., 204.)-When a mixture of alcohol and ether is distilled with a resin such as colophony, the alcohol is retained by the pasty residue left in the flask.Thus, on distilling a litre of ether containing about 1 per cent. of alcohol with about 50 grams of colophony, a distillate is obtained free from alcohol. C. A. M. Formic Acid as Preservative. G. Lebbin. (Chem. Ztg., 1906, xxx., 1009.)- From the author’s experiments it appears that the addition of 0.15 per cent. of anhydrous formic acid acts as a perfect preservative for all manner of food-stuffs, more especially fruit extracts and syrups. I n most cases 0.10 per cent. even is quite sufiicient. As regards toxic properties, reasoning from experiments on rabbits, the author finds that it would take a dose of 3.5 grams of formic acid to produoe harmful results on an adult human being.From actual experiments on himself and his assistants, he finds that a daily dose of 0.5 gram formic acid, taken regularly in the form of lemonade for two to four weeks, was without the slightest effect. He believes that it ie perfectly safe to assume that formic acid is not more than twice as poisonous as acetic acid. A. G. L. The Action and Efficacy of Preservatives. A. Behre and A. Segin. (zeit. Untenuch. Nahr. Genussm., 1906, xii., 461-467.)-Tabulated results of experiments with various preservatives are given. Definite quantities of the preservatives were added to unsterilieed meat-juice diluted with water, and observations made as to theTHE ANALYST. 405 change in colour of the solutions as well as to the time taken before an odour of decomposition was noticeable.The results show that formaldehyde has by far the most powerful preserving action, that benzoic acid is a better preservative than salicylic and boric acids, and that sodium benzoate is about equal to boric acid, whilst sodium thiosulphate and sulphite are very feeble preservatives. W. P. S. Gravimetrie Determination of Potassium Nitrate in Meat. C. Paal and G. Mehrtens. (Zeit. Untersuch. Nahr. Gewussm., 1906, xii., 410-416.)-The method described is an application of Busch’s process for the determination of nitric acid by means of ‘‘ nitron ” (see ANALYST, 1905, p. 256). Fifty grams of the finely-minced meat are agitated with warm water for about two hours, the mixture being then brought to boiling and the solution filtered. The residue is boiled out with several successive small quantities of water until the extracts no longer give a reaction with diphenylamine, and the united extracts are then diluted to a volume of 500 C.C.Two hundred C.C. of the solution are now evaporated to a volume of about 50 C.C. When quite cold, 3 drops of ammonia and a slight excess of neutral lead acetate solution are added, the mixture is boiled, again cooled, filtered, and the precipitate washed. The filtrate is acidified with acetic acid and boiled, sufficient L L nitron ” dissolved in acetic acid being added to precipitate all the nitrate present. The vessel containing the mixture is kept in ice-water for three hours, after which period the precipitate of L L nitron ” nitrate is collected on a, filter, washed with 10 to 12 C.C.of ice-water, and dried at a temperature of 110” C. The weight of the precipitate multiplied by 0-26933 gives the amount of potassium nitrate in the 200 C.C. of solution taken for the determination. Basic lead acetate must not be used for clarifying the meat decoction, as its use tends to give low results; sodium chloride, even when present in the meat in considerable quantity, does not interfere with the determination, as most of it is removed with the lead precipitate. w. P. s. The Determination of Unaltered Casein in Cheese. A. Trillat and Sawton. (Ann. de Chin?,. Anal., 1906, vol. 11, 363-365.)-The unaltered casein in cheese forms an insoluble product with formaldehyde (ANALYST, xxxi., 260), whilst the broken-down products formed from the casein as the cheese matures remain soluble.Two grams of the sample are triturated with 10 C.C. of hot water, the mixture treated little by little with 50 C.C. more of w.ater (very faintly ammoniacal water in the case of hard cheese), and boiled for five minutes. I t is next treated with 0.5 C.C. of commercial formalin, boiled for three minutes longer, and allowed to stand for five minutes, for the fat to rise to the surface. The casein is then pre- cipitated by means of 5 drops of pure acetic acid, and the precipitate collected, extracted with acetone, dried, and weighed as described in the previous communica- tion. The following percentages of casein were thus obtained with commercial samples of cheese : Camembert, 18.20 ; Gruydre, 31.34 ; Gervais, 6.41 ; Brie, 22.93 ; Roquefort (half-ripe), 11.65 ; Roquefort (very ripe), 7.10 ; and Dutch, 31.5.Tho process of ripening may also be followed, and the ratio between the amounts of original and altered casein determined. Thus a sample of fresh Roquefort cheese gave the following results : Original cheese, 19.48 ; after eight days, 18-12 ; after4Q6 THE ANALYST. fifteen days, 11.65; after thirty days, 8 ; and after sixty days, 7.10 per cent. of unaltered casein. The authors have proved by control experiments that the casein separated by this method does not contain any foreign substances, and that it has the composition of milk casein ; also that any peptones or albumoses formed are not rendered insoluble by formaldehyde. They have obtained similar results in the artificial digestion of casein with pepsin.C. A. M. On the Carbohydrates occurring in Spices. 1. In Canella Bark. J. Hanus and F. Bien. (Zeit. Untemuch. Nnlzr. Genussm., 1906, xii., 395-40’7.)- The quantity of pentosan occurring in spices is fairly constant for each kind of spice ; the largest amount (18.28 per cent. on the dry substance) being found in canella bark and the least in those spices which consist of the flowers of the plant. The quantity of crude fibre yielded by a spice is proportional to the pentosan content. The pentosans found in canella bark are not completely hydrolysed by 8 per cent. sulphuric acid, a considerable portion, closely resembling cellulose, remaining unattacked. Canella bark contains about 8 per cent.of mannite, and, on treating the bark with water under pressure, araban, galactan, and small quantities of xylan go into solution. The residue from the aqueous extraction still contains xylan and, possibly, dextrosan, these two polysaccharides dissolving when the residue is treated with 5 per cent. sulphuric acid. w. P. s. The Quantity of Tin in Tinned Tomatoes. C. Formenti and A. Scipiotti. (Zeit. Untersuch. Nahr. GenzzLssrn., 1906, xii., 290-293.)-From 0.091 to 0-128 per cent. of tin was found in six samples of tinned tomato pulp, the determinations being made immediately after the tins were opened. I n two cases the pulp was left in the tins for five days, and the tin content of the pulp again determined. I n one sample the quantity of tin increased from 0.091 to 0.324 per cent,, and in the other from 0.093 to 0.169 per cent.As Ungar (Zeit. fiir Hygiene, 1887, ii., 241), Gunther (Rec. intern. fulsif., 1887), and others have published results showing the injurious effect of tin compounds on animals, it is important that the dissolving action of fruit acids on tin should be prevented as far as possible, either by varnishing the interior of all tins in which fruits, etc., are preserved, or by removing the fruit from the tin as soon as the latter is opened. w. P. s. Determination of Cellulose, Lignin, and Cutin in ‘‘ Crude Fibre.” J. Konig. (Zeit. Untersuch. Nahr. Genussm., 1906, xii., 385-395.)-Methods have already been given for the determination of cellulose and lignin in ‘‘ crude fibre ” (ANALYST, 1903, p. 318), and it is now shown that the “cellulose” thus obtained may be further split up, by treatment with ammoniacal copper solution, into pure cellulose and cutin.The ‘‘ crude fibre ” is determined as already described, and a, second portion of the sample is treated according to the process given previously, that is, with glycerol and sulphuric acid, and afterwards with ammoniacal hydrogen peroxide. The residue obtained is, together with the asbestos filter, now treated for two hours with 75 C.C. of ammoniacal copper solution, prepared by saturating 24 per cent. ammonia with hydrated cupric oxide (Merck). The mixture is then gentlyTHE ANALYST 407 warmed and filtered through asbestos, the residue is washed with water, dried on the filter at 110’ C., and weighed. After ignition, the filter is re-weighed, the difference in the two weighings giving the weight of the cutin.Three hundred C.C. of 80 per cent. alcohol are next added to the filtrate from the cutin residue ; on stirring the mixture, the cellulose separates out and is collected on an asbestos filter, dried at llO°C., and weighed. The difference between the quantity of “crude fibre” and the sum of cellulose and cutin gives the amount of the oxidizable part of the ‘‘ crude fibre,” the so-called lignin. w. P. s. Further Simplification of the Determination of ‘‘ Pepsin-Soluble ” Nitrogen in Feeding-Stuffs. A. Stutzer, H. Wangnick, and W. Rothe. (JOZLT7L. L a m . , 1906, vol. 54, p. 365 ; through Cheiiz. Zty., 1906, xxx., Rep., 338.)- A strong extract for determining the pepsin-soluble nitrogen in feeding-stuffs is prepared by cutting up the inner mucous coat of at least six pig stomachs and allowing the fragments to stand, with occasional agitation, in 0.2 per cent.hydro- chloric acid for twenty-four hours in a cool place, 2.5 litres of liquid being taken for every stomach used. The extract obtained is filtered first through flannel and then through paper. So much chloroform is then added that a portion retnains undis- solved, and the liquid is kept in a cool place. A. G. L. Determination of Digestible Proteids in Feeding-Stuffs. A. Stutzer. (Journ. Landw., 1906, vol. 54, p. 235; through Chcqn. Ztg., 1906, xxx., Rep., 338.)- The separation of proteids from non-proteids by means of copper hydroxide has been proved to work well, both when previously prepared copper hjrdroxide or when a mixture of copper sulphate and sodium hydroxide is used.In both cases the liquid should be kept slightly acid; this may be done by adding a few C.C. of strong alum solution, or by employing an excess of copper sulphate solution. To determine “ pepsin-solubls ” nitrogen, 2 grams of the feeding-stuff are digested for forty-eight hours at blood temperature with 500 C.C. of gastric juice prepared according to the author’s old, or 250 C.C. according to his new, prescription (see preceding abstract). The amount of proteid actually digested by the animal stomach is, however, often diiferent from that indicated by the quantity of ‘‘ pepsin-soluble ” nitrogen found. A. G. L. Characteristics of Annam Beeswax. J. Bellier.(Ann. de Chim. Aital., 1906, vol. 77, pp. 366-368.)-The sample of this wax examined by the author was in the form of prismatic cakes containing 5 02 per ccnt. of water, 0.5 per cent. of substances insoluble in benzene, and 0.08 per cent. of ash. The wax itself, when melted and filtered, resembled European waxes in appearance. It gave the following results on analysis : Specific gravity, 0.964 ; melting-point, 61” C. ; acid value, 7.8 ; ester value, 86.6 ; ratio of acid value to ester value, 11 ; iodine value, 6 ; hydrogen liberated at 250’ C. by potash-lime, 60.3 C.C. per grain at 0” C. and 760 mm.; and hydro- carbons unsaponifiable at 250’ C., 10.5. The wax thus differs from European waxes in having a higher iodine value, and containing less free acids and more combined acids, so that the ratio is 11 instead of the usual 3.8.The amount-of hydrogen liberated is also much greater. On the other hand, these constants are very similar408 THE ANALYST, to those of Indian waxes, and in particular of that of Apis dorsata (see ANALYST, xxx., 57). C. A. M. The Characteristics of Essential Oil of Juniperus Phaenicea. J. Rodie. (BUZZ. SOC. Chim., 1906, xxxv., 922-925).-This oil is stated to be sold in France in place of savin oil (JzLnzperus sabinus), which it closely resembles. The pharma- ceutical and chemical differences were studied by Umney and Bennett (Pharm. Journ., lxxv., 827), who found that the substitute had a specific gravity of 0.892 at 15" C. and an optical rotation of + 4" 30' in a 100 mm. tube. Five samples of the oil of undoubted purity examined by the author had a specific gravity of 0.867 to 0.868 at 15' C., and an optical rotation of + 2" 54' to + 4" 10'.The low specific gravity of some of these samples was attributed to there being a larger proportion of terpenes in oil from younger trees and differences in the mode of distillation. Umney and Bennett found only 64 per cent, of constituents boiling below 165' C., whilst a sample distilled by the author yielded 92.3 per cent. of a, terpene fraction boiling between 154" and 180" C., nearly the whole passing over between 155" and 160" C. In addition to pinene, already identified by the English chemists, this fraction was found to contain traces of camphene and phellandrene. C. A. M. Characteristics and Reactions of Oil of Cade.C. Pepin. (Jounz. Pham. Chim., 1906, xxiv., 248-259.)- From an examination of samples of known purity the author concludes that genuine oil of cade derived from Juniperus oxycedrus should have the following characteristics : It should be fluid, have an unmistakable odour of smoke, and a, specific gravity slightly less than that of water. Its acidity, in terms of acetic mid, should be less than 1.5 per cent. When distilled under the ordinary pressure it should yield at least 65 per cent. of distillate between 150' and 300" C., and at least 70 to 75 per cent. between 10" and 215' C., on distillation under a pressure of 0.065 mm. A sample of pine-tar oil had an acidity of 1-555 per cent., and gave 15.2 per cent, of distillate between 150" and 300" C.under the ordinary pressure, and 23-2 per cent. between 10" and 215" C. under the reduced pressure. Pure oil of cade should always give a brown coloration in the test for pine-tar oil with petroleum spirit and copper acetate (ANALYST, xxxi., 302). In the author's opinion, no reliance can be placed on the colour reactions given by Hirschsohn and Adam, or in the results of the tests for furfural or pyrocatechol, which, according to Kauffeisen, are present in pine-tar oil, but not in aqueous solutions of true oil of cade. All the samples examined by the author gave the reactions for both substances. C. A. M. Determination of Minute Quantities of Morphine. C. Mai and C. Rath. (Aychiu Pharm., ccxl., 300; through Pharm. Jount., 1906, vol. lxxvii., p. 413.)- With a view of obtaining a means for determining quantities of morphine of less than 1 mgm.in weight, the authors have investigated the iodic acid reaction, the colora- tion with Frohde's reagent and that with Marquis's reagent. The latter consists of a mixture of 2 drops of 40 per cent. formaldehyde solution with 3 C.C. of sulphuric acid. Of these reactions that with Marquis's reagent was the only one that provedTHE ANALYST. 409 to be practicable. I t is carried out as follows : One C.C. of a 0.1 per cent. morphine hydrochloride solution is evaporated to dryness in a basin, and the residue mixed with 1 C.C. of the reagent. The liquid is transferred to a small test-tube, and the basin rinsed with 4 C.C. of sulphuric acid. With 0.001 gram of the alkaloid the mixture assumes a deep violet-blue colour ; with smaller quantities the coloration is less intense and is easily comparable colorirnetrically. The limit of morphine that can be determined is 0.00003 gram.TV. P. s. TOXICOLOGICAL ANALYSIS. A Simple Method of Differentiating the Blood of Different Animals. Piorkowski. (Ber. d. phaym. Ges., 1906, 226; through J0ur.n. Pharna. Cham., 1906, xxiv., 272, 273.)-The following simple method of applying the serum test for blood has been devised by the author : One C.C. of hydrocele liquid, ascites fluid, or of human serum, is introduced into each of a series of test-tubes (6 c.m. long by 0.8 c.m. in diameter), then one drop (0.04 c.c.) of the fresh blood of different animals diluted ten to fifty times, or better, of the dried blood previously dissolved in a physiological solution of salt. Hydrocele fluid forms the best reagent, and the blood must be allowed to fall from the pipette so as to form a layer on the surface of the other liquid. The tubes are examined thirty to forty-five minutes after the introduclion of the blood, and if the latter is of human origin a faint red precipitate (of coagulated blood) will be observed, while the supernatant liquid will have remained clear. On the other hand, the blood of other species will have dissolved in the human serum, colouring it red. If the tubes are charged, in the first place, with serum of the horse, ox, or other animal, the corresponding blood is coagulated, while chat of any other animal dissolves. The reactions are rendered more conclusive by cautiously shaking the tubes every half-hour after the coagulation has taken place, a fresh precipitate being formed each time. In preparing the solution of blood, the action of the sodium chloride (or sodium carbonate) upon the stain, etc., iff continued until the liquid is manifestly yellow, aftcr which it is filtered and tested as described. C. A. M.

 

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