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Foods and drugs analysis

 

作者:

 

期刊: Analyst  (RSC Available online 1904)
卷期: Volume 29, issue December  

页码: 370-375

 

ISSN:0003-2654

 

年代: 1904

 

DOI:10.1039/AN9042900370

 

出版商: RSC

 

数据来源: RSC

 

摘要:

370 THE ANALYST. ABSTRACTS OF PAPERS PUBLISHED IN OTHER J 0 U R N ALS. FOODS AND DRUGS ANALYSIS. The Influence of Various ‘‘ Fining ” Materials on the Composit,ion of Wine. K. Windisch and T. Roettgen. (Zcit. Untersuch. Nahr. P L ~ Gemm?uittd, 1904, viii., 279-283.)--Analyses are given of wines both before and after the latter had been treated with “fining” materials, such as casein, milk, wood charcoal and animal charcoal. The results show that casein slightly increases the amount of mineral matter in the wine, but is without influence on the tannin and nitrogenous matters. Milk also slightly increases the quantity of mineral matter present in the wine, whilst it removes a considerable portion of the tannin, owing to the albumin it contains. By treating wine with animal charcoal, a distinct diminution in the amount of tannin takes place, but no nitrogenous matters are precipitated.Wood charcoal only slightly diminishes the tannin contents of the wine; it increases the mineral matter to a small extent, but is without influence on the nitrogenous matter. The assumption that “ fining ” materials considerably alter the composition of wines is probably dueTHE ANALYST, 371 to the very bulky sediment which is obtained. Experiment shows that a solution 0.01 gramme of casein, added to 100 C.C. of wine, produces a voluminous precipitate, which settles to form a layer of appreciable thickness. This precipitate, however, weighs but little more than 0.01 gramme. w. P. s. Margarine containing Ammonia. K. Fischer and 0. Grunert. (Zeit.Unter- such. Nahi.. u?zd GeTzzLssmittel, 1904., viii., 414-416.)-During the examination of a sample of margarine, it was noticed that the aqiieous layer obtained on melting the sample was strongly alkaline in its reaction. This alkalinity was due to the presence of ammonia, the quantity of the latter contained in the margarine being 0.017 per cent. I n other respects the sample was of normal quality. Further tests showed that no appreciable amount of the ammonia was c.ombined with fatty acids, w. P. s. the probability being that it was present as the carbonate. Quantitative Estimation of Cellulose in Foods and Faeces. Oscar Simon and Hans Lohrisch. (Zeit. Phys. Chem., 1904, xlii,, 55 ; through Chem. Zeit. Rep., 1904, xxi., 254.)-This process is based upon the insolubility of cellulose in 50 per cent.potash solution. Ten grammes of the finely-powdered substance are heated on a water-bath for one hour with 50 per cent. KOH. After cooling, 3 to 4 C.C. of hydrogen peroxide are added, and, if necessary, further heated until the greater part of the cellulose is in solution. The mixture is again cooled, one-half volunie of 96 per cent. alcohol added; should the mixture of the liquids not be complete, 6 to 7 C.C. of concentrated acetic acid are added, Precipitation of the dissolved cellulose is complete ; proteids, etc., remain in solution. When cold the precipitate is filtered off, thoroughly washed with water and dilute acetic acid, finally with alcohol and ether, and weighed. The nitrogen never exceeds 1 per cent. The nature of the cellulose has great influence on its solubility ; potato cellulose is largely soluble, wheat cellulose less so, while prepared celluloses, as cotton or filter-paper, are quite insoluble.H. A. T. The Proteids of Wheat Gluten. J. Konig and P. Rintelen. (Zezt. Unter- such. Nahr. 7cnd Geizussnaittel, 1904, viii., 401-407.) - The following method is proposed for the separation of the various proteids extracted from gluten by 65 per cent. alcohol. Of these, a portion, the so-called gluten-fibrin, is soluble in 90 per cent. alcohol; another portion, mucedin, is soluble in 40 per cent. alcohol, whilst gliadin is insoluble in the latter spirit. Gluten-casein is practically insoluble in any of these alcoholic solutions. The details of the method are as follows: 2 to 3 grammes of the washed gluten are moistened with absolute alcohol and finely divided, after which the mass is treated in a cylinder with alcohol and ether to remove fat.The small amount of proteid dissolved by the absolute alcohol is precipitated on adding the ether, and is collected and added to the cake of gluten. The latter is now placed in a linen bag, suspended in a cylinder, and covered with 65 per cent. alcohol. The The gluten is then lightly pressed, air-dried, and again powdered.372 THE ANALYST. solvent is frequently renewed, a considerable quantity-several litres-being used for the extraction. To the clear alcoholic extract obtained sufficient absolute alcohol is added to bring the alcoholic strength up to 90 per cent. A white precipitate is obtained, which may be made to settle or collect together by cooling the solution in ice-water and shaking.After filtration, the filtrate is evaporated, the residue, which also contains sugars and fat, is rubbed down with water, again dried, and extracted with ether. The residue of gluten-fibrin so obtained may still contain a little fat. To remove this, the mass is dissolved in dilute alcoholic potash, the solution shaken out with ether, and the alkaline solution exactly neutralized with hydrochloric acid and evaporated. The precipitate, consisting of gliadin and mucedin, obtained from the 90 per cent. alcohol solution, is dissolved in 65 per cent. alcohol, using sufficient of the latter to form a practically saturated solution. One-half the alcohol is now distilled off', and the residual liquid allowed to cool.Gliadin separates out and adheres to the sides of the flask. The clear solution is poured off and evaporated to two-thirds its original volume. On cooling, a mixed precipitate of mucedin and gliadin is Obtained, which is rejected. The clear solution separated from this precipitate, on evaporation, yields a residue consisting of mucedin. Analyses of these three proteids, separated from various glutens, are given. From the differences in their compositions, and in their solubilities in alcohol, the author concludes that they are actually three separate compounds and not one, as has been suggested by other observers. w. P. s. Detection of Artificial Colouring Matters in Mustard. P. Bohrisch. (Zezt. Uiztersmh. Nahr.uizd Geimssnzittcl, 1904, viii., 285, 286.)--The usual test for aniline colours, consisting in steeping woollen threads in a solution of the substance under examination, fails in the case of mustard. Kven pure samples dye the threads yellowish, the coloration becoming almost bright yellow on treatment with ammonia. If, however, the dyed woollen threads be washed with water, all the yellow colora- tion is removed, should the sample consist of genuine mustard. When aniline colours are present, the bright yellow colour remains. . The presence of turmeric in mustard may be detected by treating 10 grammes of the dry sample with 30 C.C. of absolute alcohol, allowing the mixture to stand for twelve hours, and then filtering. Strips of filter-paper are partially immersed in the alcoholic filtrate, and the yellow zone obtained is tested with boric acid solution.Should turmeric be present, the characteristic red coloration is obtained on dyeing the strip. Pure mustards give a yellowish-brown to gray-brown band on the strip of paper. w. P. s. Alteration i n the Composition of Asparagus when stored in Water. E. Windisch and P. Schmidt. (Zed. U I ~ ~ C I . S Z L C ~ . N ~ L Y . und Geizussmittel, 1804, viii., 352-355.)-As cut asparagus rapidly loses its freshness when kept, it is a market custom to store it in water in a dark cellar. To ascertain what changes take place during this treatment, the authors carried out a number of experiments.THE ANALYST. 373 Saponifica- tion T'alue. The results show that the asparagus absorbed a considerable amount of water- 12.16 per cent.in five days-whilst at the same time some of its constituents were dissolved out. I n five days 5.02 per cent. of the extractive matters, 6.30 per cent. of the nitrogen, and 8-36 per cent. of the mineral matters contained in the original asparagus were extracted by the water. By coating the cut surfaces of the sticks with paraffin the extraction was considerably diminished, but the absorption of water by the asparagus was not affected. When kept in the open air in a cool room the asparagus lost 23.10 per cent. of water in six days. Stored for the same time in an ice chest, the loss only amounted to 9.68 per cent. w. P. s. Essential Oil, l'er Cent. Refractive Index of Clove Oil. W. H. Simmons. (Chem. News, xc., 146.)- The author recommends the determination of the refractive index, together with the specific gravity and percentage of phenols, in the examination of clove oil.The refractive index for pure oils is approximately proportional to the amount of eugenol present, for which n,20" = 1.5412. A. G. L. Very pale yellow Yellowish-brown Pale yellow Yellowish-brown With greenish tint Pale yellow >, Copaiba Balsam from Surinam. L. van Itallie. (Jozmz. Pharm. C h k , 1904, xx., 337-346.)--hccording to Pool, this balsam is always very fluid when fresh, and thick products are due to resinification or adulteration. Seven samples examined by the author gave the following results : Very fluid Syrupy Very fluid Syrupy - - Very fluid Sample. A ... B ... c ... D ... E ... F ... G ...Colour. Consistency. Specific 0.9066 0.9599 0.9096 0.9611 0.9600 0.9535 Acid Talue. 15.7 59.19 14-65 59 a00 33.8 53.5 - 26.1 77.4 25.2 75-8 45.4 43.2 - ~ 69.1 42.3 71.6 41.0 52.3 61.7 - The essential oil was determined by heating the balsam on the water-bath and finally in the oven at 110" C. The balsam is not completely soluble in 5 parts of absolute alcohol, but dissolves readily in chloroform, petroleum spirit and carbon bisulphide. When shaken with a third of its volume of 10 per cent. ammonia solution, an emulsion is formed, from which, on stand- ing, drops of essential oil separate. On shaking the Surinam balsam with an 80 per cent. solution of chloral hydrate, the essential oil separates out on the surface, but the solution of the resin does not assume a special colour, such as Blauch found to be the case with Gurjun balsam.A very characteristic reaction for the Surinam balsam is the blue coloration obtained on adding a drop of sulphuric acid to a mixture of 1 drop of the balsam with 1 C.C. of acetic anhydride. The essential oil was found to contain a sesquiterpene alcohol (C,,H,,O) giving the reactions of cholesterol derivatives, a small amount of cadinene, and at least two374 THE ANALYST. sesquiterpenes. The liquid portion of the essential oil, after separation of the alcohol crystals, was a viscous liquid, which became light yellow on standing. It had the following characteristics : Specific gravity at 15" C.,* 0.9052 ; saponification value, 6.7; acetyl value of saponified oil, 28.4; and specific rotation, a,,= -10.3 in 100-millimetre tube.When distilled under normal pressure, the principal part passed over between 240" and 270" C., only a few drops distilling below 240" C. Between 2'70' and 280" C. a small amount of a pale-green empyreumatic product was distilled, whilst the residue in the flask was a dark-brown substance which solidified on cooling, and dissolved in ether, forming a solution with a strong green fluor- escence. C. A. M. Some Colour-Reactions of Strychnine and Brucine. C. Reichard. (Chem. Zeit., 1904, xxviii., 977-979.)-The following reactions are described : On adding a drop of a solution of a strychnine salt to a drop of dilute solution of cupric nitrate and evaporating the mixture, the edges of the solution as it dries become deep green in colour ; the addition of stannous chloride to the dry residue changes the green colour to4 violet, which latter coloration again beconies green when dry.A solution of strychnine nitrate treated with a drop of platinum chloride and concentrated sulphuric acid gives a, dark-red coloration on warming the mixture ; brucine similarly treated gives a yellow coloration. When drops of hydrogen peroxide, a solution of strychnine, and sulphuric acid are mixed, a blue solution is obtained having yellow edges. After a time the blue colour changes to yellow ; ether does not dissolve this latter colouring matter. Sulphuric acid, strychnine, and titanic acid yield, on warmiiig, a blue coloration, changing to yellow on standing or further heating, and a similar coloration is obtained with the same reagents in the case of brucine, but the addition of water discharges the colour, whilst the strychnine coloration remains yellow on dilution.A drop of a solution of a strychnine salt mixed with potassium hydroxide and evaporated gives a residue, which is turned blue by stannous chloride ; brucine similarly treated yields no coloration. Solutions of strychnine, when mixed with potassium or ammonium persulphate and hydrochloric acid, remain colourless, whilst brucine gives a bright-red coloration, only becoming colourless after I a long time. This last reaction is very useful for detecting the slightest trace of brucine in solutions of strychnine. On heating, the strychnine mixture turns yellow. w. P. s. A New Method for the Detection of Saccharin.E. von Maler. (Farmax. JOWL, 1904, 1089 ; through Chenz. Zeit. Rep, 1904, xxii., 270.)-Schmidt's method, in which the sulpho group of the saccharin is replaced by a hydroxyl group by fusion with caustic alkali, and the resultant potassium salicylate detected by ferric chloride, is unsatisfactory. Not only must the temperature of fusion be care- fully regulated, but the presence of any salicylic acid in the substance would also render the reaction inaccurate. 15" 15 * Probably Ls, Init w.iLtcr teniperature not given.TEE ANALYST. 375 The author fuses the substance with metallic potassium or sodium, converting the sulpho group into sulphides, which can be detected by sodium nitroprusside. H. A. T. Report and Itecommendations with Reference t o the Tests for the Detection of Arsenic in the Drugs of the British Pharmacopmia.W. R. Dunstan and H. H. Robinson. (Presented to the Phawn. Committee of the Gen. Med. Co~c?aci~, May, 1904.)-The results of investigations regarding the validity of the present tests for arsenic, and the best processes to be adopted in the next edition of the British Pharmacopceia, are given in this report. With the desire that the standard process should be such as could readily be applied by a qualified pharmacist without com- plicated apparatus, the test chosen is that proposed by Mayenqon and Bergeret (Comptes Rend., 1874, lxxix., 118), which depends on the production by arseniuretted hydrogen of a stain on paper soaked in mercuric chloride. The Marsh-Berzelius test was excluded, as requiring complicated apparatus, extreme purity of the reagents employed, and continuous attention during its performame. Precise instructions are given for carrying out the test recommended, and for its application to certain drugs. The stain decided on as the standard for comparison, and as showing that a drug contains an inadmissible amount of arsenic, is that given by 0.012 milligramme of the element arsenic, which is equivalent to 0-016 milligramme of arsenious oxide. The limiting quantity of arsenic which should be regarded as rendering a drug impure is fixed at 3 parts of arsenic per million, or :& grain of arsenious oxide per pound. This limit applies only to drugs administered in small doses. Tartaric and citric acids should not contain more than & grain of arsenic per pound. The following limits are proposed for drugs which are not readily freed from arsenic in their manufacture : Iron, 0.03 per cent. ; antimony sulphides, 0.03 per cent. ; phosphorus, 0.02 per cent. Ferrous sulphate, and those iron drugs which are made from it, fall under the general limit, as they can be obtained free from arsenic. w. P. s.

 

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