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Foods and drugs analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1906)
卷期: Volume 31, issue 364  

页码: 227-235

 

ISSN:0003-2654

 

年代: 1906

 

DOI:10.1039/AN9063100227

 

出版商: RSC

 

数据来源: RSC

 

摘要:

THE ANALYST. 227 ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. (Zeit. UfentZ. Chem., 1906, xii., 167, 168.)-A preparation, sold to confectioners, under the name of artificial milk, has recently been examined by the author and found to consist essentially of sesame oil, sugar, and albumin. Milk Substitute, R. Racine. The results of the analysis were : Total solids ... ... ... ... ... 85-90 per cent. Ash ... ... .., ... ... ... 0.16 ,, Oil (sesame) ... ... ... ... ... 47.10 ,, Sugar (as invert sugar) ... ... ... 34.00 ,, Albumin ... ... ... ... ... 4-51 ,, The preparation was of a syrupy consistency, and, when mixed with water in any proportion, gave milky solutions from which the oil separated very slowly. w. P. s. Adulteration of Butter with Casein.R. Racine. (Zeit. oflentl.. Chein., 1906, xii., 169-170.)-A sample of butter was found by the author to have the following composition : Fat, 69-01 per cent. ; water, 24.73 per cent. ; ash, 0.77 per cent. ; casein, 5.49 per cent. This form of adulteration is readily detected owing to the large quantity of coagulum obtained on melting the sample. It will also be seen that an excessive quantity of water was contained in this butter. w. P. s. The Detection of Bleached Flour in Wheat Flour. E. Fleurent. (Compte.9 RE~C~US, 1906, cxlii., 180 ; through Jour~z. Pharm. Chinz., 1906, xxiii., 499, 5OO.)-Thc228 THE ANALYST, only processes of bleaching flour that have an industrial value are those in which nitrogen peroxide is used as the reagent. Pure oxygen or ozone.does not affect tbe colour, and although ozonized air has a, bleaching effect, it is only when it is simul- taneously charged with nitrous products.Moreover, flours treated with ozone acquire a repulsive odour, which destroys their commercial value. The quantity of nitrous vapours in terms of nitrogen peroxide absorbed ranges from about 15 to 40 C.C. per kilogm. of flour. The nitrogen peroxide forms an addition compound with the fat, the iodine value of which is correspondingly lowered. The action of ozone, however, causes an increase in the iodine value and the formation of volatile fatty acids. The fixation of the nitrogen peroxide by the fat affords a means of differentiating bleached from normal flour. Fifty grams of the sample are extracted with petroleum spirit (benzine), the extract evaporated at a low temperature, the residue of oil dissolved in 3 C.C.of amyl alcohol, and the solution shaken with 1 C.C. of a 1 per cent. alcoholic solution of potassium hydroxide. In the case of a normal flour the resulting soap solution is of the same pale yellow colour ; but when the flour has been bleached the colour changes to reddish-orange, the depth of shade depending upon the amount of nitrogen peroxide that had been fixed by the fat. The test is capable of detecting the addition of 5 per cent. of bleached flour to ordinary flour, The bleaching process has no action upon the diastase or other enzymes of the flour, but the fat becomes acid more slowly than that which has not combined with nitrogen peroxide. I t is in this sense only that the bleaching process can be said to have any preservative action upon the flour.C. A. M. A Study of the Proteids of Beef-Flesh. P. F. Trowbridge and H. S. Grindley. (Journ. Anzer. Chem. SOC., 1906, xxviii., 469-505).-The results of their previous work (ANALYST, 1905, 89) led the authors to the conclusion that much additional information regarding the proteids of flesh could be obtained by extracting the flesh successively with cold water, with a 10 per cent. ammonium sulphate solution, and finally with & potassium hydroxide solution in the cold. An investi- gation on these lines was therefore carried out, together with a study of the acidity of the flesh, with the following results: The total acidity of aqueous extracts of flesh varies between comparatively wide limits, the minimum being 0.66 per cent., the maximum 1.07 per cent., and the average 0.85 per cent., calculated as lactic acid and expressed in terms of the fresh meat.Whilst the residues of flesh which are left after complete extraction with cold water are distinctly acid to litmus and to phenolphthalein, the insoluble proteids of flesh upon digestion with 2c hydrochloric acid, at the ordinary temperature, combine with the latter, neutralizing its acid properties. The analyses show that 13.56 per cent. of the total proteids existing in lean flesh is soluble in cold water. Of this, 90.04 per cent. is coagulable by heat from a neutral solution, 840 per cent. exists in the form of albumoses, and a very small quantity apparently as peptones.It is not at present supposed that the albumoses and peptones exist as such in the original flesh, During the coagulation of an aqueous extract of flesh there is an increase in the acidity of the same. Reduction of the acidity of the extract facilitates the coagulation of the proteids, the separationTHE ANALYST, 229 of the coagulable proteids being more complete with one-fourth neutralization (to phenolphthalein) of the acidity of the extract than it is on further neutralization. The partial neutralization of such extracts causes the precipitation of some proteid matter at the ordinary temperature. There is no well-defined temperature at which different coagula of flesh extracts separate. The complete removal of the proteid coagulating at any definite temperature requires long application of heat , and the lower the temperature at which a coagulum is separated, the longer the time required to effect the separation.Of the total proteid of a cold water extract of flesh, 11-71 per cent. is separated by neutralization, 36.65 per cent. is coagulable below 50" C., 39.99 between 51" and 75" C., and 11.71 between 76" and 85" C. The chemical composition of the different fractional coagula is remarkably constant, and, judging from the results of their hydrolysis, their chemical constitutions are quite similar. Raw flesh which has been completely freed from proteids soluble in cold water contains two classes of proteid substances-those which are soluble in 10 per cent. ammonium sulphate solution and those which are insoluble, Of the total proteids of lean flesh about 16 per cent.are insoluble in cold water, but soluble in 10 per cent. ammonium sulphate solution. The latter solution extracts from flesh at least two individual proteids or groups of proteids which differ in physical properties, and to some extent in chemical composition. The residue left after extracting raw flesh with cold water and 10 per cent. ammonium sulphate aolution is almost entirely soluble in & potassium hydroxide solution, and has the same chemical composition even when separated from the solvent by different means and purified by widely different treatment. w. P. s. The Presence of Sodium Arsenate in Preserved Meat. A. Andouard. (Journ. Pharm. Chiin., 1906, xxiii., 417,418.)--Sodium nitrate has gradually replaced potassium nitrate as a means of giving to preserved pork the rosy colour of the fresh meat.In the author's opinion, it is less injurious than nitre, but he considers that the use of any alkaline nitrate for such purposes should be prohibited, both on account of their active medicinal properties and of the risk of poisoning from the use of impure salts. Several 'instances of such poisoning have come under his notice, and in three cases the supposed sodium nitrates used for colouring the flesh were found to contain sodium arsenate. C. A. M. Determination of Fat Oin Cocoa. A. Kirschner. (Zeit. Untersuch. Nnhr. Genussm., 1906, vol. 11, pp. 450, 451.)-The following manner of applying the Gottlieb process (ANALYST, 1898, 259) to the determination of fat in cocoa is described : A weighed quantity of about 1.5 grams of the cocoa and SO C.C.of alcohol (50 per cent. by volume) are shaken together in a graduated cylinder. The latter should have a capacity of 75 or 100 c.c., be divided into divisions of 0.5 c.c., and be of such a diameter that the height between the 0 and 75 C.C. marks is not less than 30 cm. ; 25 C.C. of ether are then introduced, and the mixture shaken for fifteen minutes, when 95 C.C. of petroleum spirit are added and mixed by carefully inverting the cylinder230 THE ANALYST. a few times. The cylinder is now set aside for one hour to allow the solvent to separate, 45 C.C. of the ethereal layer being then withdrawn, evaporated, and the residue of fat weighed. As the presence of the cocoa prevents the total volume of the solvent being read off, a blank experiment is made, in which the above-mentioned quantities are used, but the cocoa omitted, and the volume thus ascertained.To the total volume found in this manner is added the weight of fat obtained, 1 C.C. being added for each gram. The amount of fat in the cocoa is then found by a simple calculation. From the results given the process Care must be taken not to form an emulsion. appears to be trustworthy. w. P. s. The Determination of Foreign Substances in Cocoa and Chocolate. F. Bordas and Touplain. (Comptes Reizdus, 1906, xlii., 794 ; through Journ. Pharvz. Chirn., 1906, xxiii., 502, 503.)-Foreign substances are usually searched for with the microscope in the insoluble residue left after extraction of the fat with ether and of the sugar with water.To simplify the process, the authors have devised a mechanical method of separating the different substances by treating the residue successively with mixtures of carbon tetrachloride and petroleum spirit (benzine), ranging in specific gravity from 1,340 to 1.600. Preliminary experiments have shown that the different substances that may be in the insoluble residue behave as follows on treatment with the different mixtures : Specific Gravity. Insoluble Residue of- 1.340 ... ... Arachis cake 1.435 ... ... 9 , 1.400 ... ... Cocoa germs 1.440 9 , 1.440 ... ... Pure cocoa 1.500 ... ... 1.500 ... ... HUE& 1.530 ... ... 1.510 ... ... Piiato starch 1.525 ... ... $ 9 1.600 ... ... Mineral matter ... ... Be haviour .... ".. Sinks ... ... Floats ... ... Sink ... ... Float ... ... Sinks ... ... Floats ... ... Sink ... ... Float ... Sinks ... ... Floats ... ... Sinks ... C. A. M. A Reaction of Theobromine. G. Gerard. (Journ. Pharrn. Chim., 1906, xxiii., 476, 477.)-A small quantity (0.05 gram) of the alkaloid is mixed with 3 C.C. of water and 6 c.c: of sodium hydroxide solution (Zessive des savomiers), and the tube allowed to stand until the liquid becomes clear, after which 1 C.C. of ammonium hydroxide and 10 C.C. of a 10 per cent. solution of silver nitrate are introduced. The mixture on shaking forms a colourless transparent mass, which becomes fluid at 60" C., and sets to a transparent jelly when cooled again. If the heating be done too rapidly, too concentrated solutions of the alkaloid yield opaque jellies.I n the author's opinion, the reaction is probably due to the formation of a silver precipitate of theobromine in a gelatinous state similar to that of precipitated silica. Caffeine does not give the reaction. The test is very sensitive, and it is possible to obtainTHE ANALYST. 231 evident solidification with 0.01 gram of theobromine in 10 C.C. of liquid. When once formed, the jelIy can be kept for several weeks without undergoing any alteration. C. A. M. Detection of Sugar in Mace. E. Spaeth. (Zeit. Unterszcch. Nahr. Genussm., 1906, vol. 11, pp. 447-450.)-Notwithstanding the fact that mace contains naturally a small quantity of sugars (c$ ANALYST, 1905,207), the presence of added sugar may be detected by the following test, described by the author some years ago (1896) : Ten grams of the sample, previously freed from fat by means of petroleum spirit, are shaken with chloroform and allowed to settle.After decanting the greater part of the latter, the last few c.c., together with the sediment, are evaporated on the water- bath, and the residue dissolved in a little warm water. The solution is clarified by the addition of lead acetate and aluminium hydroxide (the latter alone is usually sufficient), diluted to 50 C.C. with water, filtered, and the filtrate examined by the polarimeter. When thus treated pure samples of mace yield no polarizing substances, and, consequently, the presence of added sugar is readily detected. w. P. s. The Ash of Pepper and Cinnamon. H. Luhrig and R.Thamm. (Zeit. Uizterszuh. Nahr, Genussm., 1906, xi., 129-134.)-The following results were obtained on the analysis of specimens of Malabar, Tellicherri, and Singapore peppercorns, 9 samples in all being examined. The figures represent percentages on the sand-free dry substance. The amount of sand present varied from 0.040 to 0-265 per cent, : ALKALINITY OF ASH : C . C . N ACID PER 100 GRAMS OF PEPPEK. ASH. >-- c A \ MTater- Water- Water- Water- Total. soluble. insoluble. Average ... 5.02 3-19 1.83 52.4 26.2 26-1 Lowest ... 4.67 2.46 1-49 49.1 15.7 20.5 soluble. insoluble. Total. Highest ... 5.60 3.57 3.14 54.9 28.6 38.3 Average ... 5.28 1.56 4-72 92.2 14.7 77.5 Eight samples of Ceylon cinnamon gave the following results : Highest ... 5-96 1.84 4.32 104.5 18.1 88.6 Lowest ...4.30 1-26 3.00 72.9 11.0 70.5 under : Two samples of cassia bark-a common adulterant of cinnamon-gave results a s 1. 2.36 0.90 1.46 34.5 5.95 28.6 2. 2-37 0.96 1.41 35.6 6.14 29.4 For the determination of the soluble alkalinity of the ash, the latter, after being weighed, was washed into a 100 C.C. flask with about 50 C.C. of water, boiled for ten minutes, then cooled and made up to the mark. The solution was filtered, and 50 C.C. of the filtrate boiled with the addition of an excess of $ N acid. The excess of the latter was then titrated back with t N alkali solution. The whole of the contents of the 100 C.C. flask were now brought on to the filter, washed with a large volume of boiling water, and the insoluble ash determined as usual. The samples of cinnamon contained very little sand--viz., from 0.02 to 0.08 per cent.w. P. s.232 THE ANALYST. The Detection of Soap-Wort in Mineral Waters. J. Vamvakas. (Ann. de Chim. anal., 1906, vol. 77, 161-163.)-A decoction of soap-wort root (Saponaria OficinaZis) is a common addition to mineral waters, and various preparations con- taining it are used to produce frothing when the bottle is opened. One of these, of English origin, examined by the author, was sold under the name of “Liqueur Lautain.” It was a, brown liquid with an odour of banana, an acid reaction, and a density of 1.140 at 15” C. It consisted, in the main, of an aqueous extract of soap- wort root, and contained 1.6 per cent. of sugar. When diluted with water, boiled, cooled, and treated with a few drops of Nessler’s reagent, it gave a bright yellow to deep orange-coloured precipitate, which became greenish-gray after a few hours, and finally leaden-gray.A similar reaction was obtained with decoctions of soap-wort root and with mineral waters containing it. If the liquids were boiled after the addition of the Nessler’s reagent, a gray precipitate, changing immediately to blackish- gray and greenish-gray, was formed. The addition of a few drops of nitric acid or of a concentrated solution of tartaric acid prevented the formation of aoy precipitate by the reagent. The following method of applying the test to lemonade and other mineral waters is recommended : 100 C.C. of the liquid are boiled to expel the car- bonic acid and the free ammonia in the water, diluted to the original volume again, and treated with lead subacetate.The white precipitate is filtered off, sus- pended in water, and decomposed with a current of hydrogen sulphide, abundant frothing being produced if the original liquid contained soap-wort extract. The liquid is now filtered, and the filtrate and washings boiled until quite free from hydrogen sulphide, cooled, and divided into three parts. One of these is tested with Nessler’s reagent and allowed to stand, the second boiled with the reagent, and the third tested with a few drops of 8 concentrated solution of tartaric acid in the hot as well as in the cold sdution. If the drink contained soap-wort, a yellow precipitate will be obtained in the first case, a greenish or grayish-black precipitate in the second, and no precipitate at all in the third. The reaction is not applicable to sparkling wines or to beer.C. A. M. The Acids occurring in Raspberry Juice. R. Kayser. (Zeit. ofentZ. Chem., 1906, xii., 155, 156.)-The following organic acids were detected and their quantity determined in (1) a sample of raspberry syrup, and (2) raspberry juice preserved with alcohol. The figures express grams per 100 C.C. after allowing for the amounts of sugar and alcohol respectively present : 1. 2. Tartaric acid . . . ... ... ... 0.220 0.180 Citric acid ... ... 0.756 0.655 Malic acid (by difference) . . . ... 0.220 0.300 Volatile acid (as acetic) ... ... 0.060 0.045 w. P. s. Composition of Raspberry Juice. Hefelmann, P. Mauz and F. Muller. (Zeit. offentl. Chem., 1906, xii., 141-155.)-The average results of the analyses of fifty samples of 1905 raspberry juice were found to be as follows :I 00.2F 16.9 42.0 96*9Z 96.9Z 4I.LC234 THE ANALYST, acetate (2 molecules of mercuric acetate to 1 molecule of camphene).The crystalline precipitate formed after thirty days’ contact is readily purified owing to its insolu- bility in most neutral solvents, and the camphene can then be recovered by means of hydrogen sulphide. C. A. M. The Lemon-scented Ironbark and its Essential Oil. R. T. Baker and H. G. Smith. (Pham. J O Z L ~ , 1906, vol. 76, pp. 571, 572.)-This small tree (Eucalyptus staigeriana) which is only at present found in Queensland, is a species with distinct characteristics and is not easily confounded with any other eucalyptus.The leaves examined by the authors yielded 2.484 per cent. of essential oil, having a light lemon colour and an odour of citral and geraniol. The rotation of the oil in a 100 mm. tube was - 43-1 ; the specific gravity at 16” C. was 0.8708, and the refractive index at the same temperature 14871. The approximate composition of the oil was: Limonene, 60.00; geraniol, 12.72; geranyl acetate, 8.32; citral, 16.00; undetermined, 2.96 per cent. From the physical properties of the fractions obtained on distillation, it is seen that nearly the whole of the terpene present was h v o - limonene. w. P. s. Peru Balsam Oil. Haensel. (HaenseZ’s Report, 1906 ; through Pharm. J O Z L T ~ . , 1906, V O ~ . 76, p. 642.)-Genuine balsam contains about 30 per cent. of essential oil which is dark yellow in colour, has a slight dextro rotation, and a specific gravity of 1.083 at 25’ C.The amount of cinnamein in this oil is 84.4 per cent. w. P. s. Determination of Camphor in Camphor Liniment. J. Lothian. (Pj2a?..~12. J0211”12., 1906, vol. 76, pp. 493, 494.)-Results of analyses are given showing that the camphor is completely volatilized from camphor liniment by heating a thin layer of the latter in a shallow, flat-bottomed basin for one hour on the water-bath. The size of the basin employed should be such that about 4 grams of the oil form a layer in it 1 mm. in depth. Under these conditions the olive oil itself does not gain in weight, w. P. s. On a Reaction of Morphine. C. Reichard. (Pham. Centralh., 1906, xlvii., 247 ; through Chenz.Zeit., 1906, xxx. [Rep.], 142.)-The formaldehyde reaction for morphine is usually carried out in the presence of concentrated sulphuric acid ; the author finds it better to add a trace of stannous chloride instead of the acid. As modified t h s , the reaction is a delicate test for either morphine or tin. A. G. L. A New Reaction of Morphine. D. Radulescu. (Bull. SOC. Sci. d. Buczmsci, 1905, 14, 602 ; through Pharm. Journ., 1906, vol. 76, p. 501.)-The following colour reaction is stated to be peculiar to morphine : A filtered decoction of the substance to be examined, as free as possible from colour, is treated with a crystal of sodium nitrite and sufficient acid to liberate the nitrous acid. Before effervescence has ceased an excess of potassium hydroxide solution is added. I n the presence of morphine a pale rose to ruby-red tint develops, according to the amount of morphineTHE ANALYST. 235 present. The kind of acid employed is immaterial, and any alkali may be used. The red colour is not removed by shaking with immiscible solvents nor discharged by boiling the alkaline solution, but is decomposed by strong acids. It also decom- w. P. s. poses in the presence of much alcohol. On the Precipitation and Quantitative Determination of Alkaloids by means of Solutions of Potassium Bismuth Iodide. D. Jonesen. (D. ~ I Z ~ L T T ~ Z . Ges. Ber., 1906, 130; through Chem. Zeit., 1906, xxx. [Rep.], 156.)-Thorns has shown that potassium bismuth iodide may be used, not only to detect organic bases, but also for the precipitation of certain alkaloids. The reagent is added to a sulphuric acid solution of the alkaloid, and the precipitate washed with dilute sulphuric acid. From the precipitate the alkaloid may be recovered by treatment with a mixture of sodium carbonate and hydrate (which treatment requires t o be prolonged in some cases). In this way, from 1 gram each of quinine, caffeine, and antipyrin, 0.9405, 0.9546, and 0.9273 gram respectively was recovered, showing the precipitation with the potassium bismuth iodide reagent to be fairly compIete. A. G. L.

 

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