Wool fat, hydrogenated EUROPEAN PHARMACOPOEIA 5.0 Sulphated ash (2.4.14) : maximum 0.15 per cent. Ignite 5.0 g and use the residue to determine the sulphated ash. Saponification value (2.5.6) : maximum 8.0. Heat under reflux for 4 h. Fatty alcohols and sterols. Gas chromatography (2.2.28). Test solution. Dissolve 0.25 g of the substance to be examined in 60 ml of ethanol R and dilute to 100.0 ml with the same solvent. STORAGE At a temperature not exceeding 25 °C. Reference solution (a). Dissolve 0.25 g of hydrogenated wool fat CRS in 60 ml of ethanol R and dilute to 100.0 ml with the same solvent. LABELLING The label states, where applicable, the concentration of added butylhydroxytoluene. Reference solution (b). Dissolve 50 mg of cetyl alcohol CRS and 50 mg of stearyl alcohol CRS in 60 ml of ethanol R and dilute to 100.0 ml with the same solvent. Column : 01/2005:0969 — material : fused silica, — size : l = 30 m, Ø = 0.25 mm, WOOL FAT, HYDROGENATED — stationary phase : poly(dimethyl)siloxane R or another non-polar phase (film thickness : 0.25 µm). Adeps lanae hydrogenatus Carrier gas : helium for chromatography R at a pressure of 100 kPa DEFINITION Mixture of higher aliphatic alcohols and sterols obtained from Temperature : the direct, high-pressure, high-temperature hydrogenation of wool fat (0134) during which the esters and acids present are reduced to the corresponding alcohols. It may contain butylhydroxytoluene. Column CHARACTERS Appearance : white or pale yellow, unctuous substance. Solubility : practically insoluble in water, soluble in boiling alcohol and in light petroleum. Time (min) Temperature (°C) 0-5 100 5 - 45 100 → 300 45 - 60 300 Injection port 325 Detector 350 Detection : flame ionisation. IDENTIFICATION Injection : 1 µl. First identification : B. Second identification : A, C. The chromatogram obtained with the test solution does not differ significantly from the chromatogram obtained with A. It complies with the test for melting point (see Tests). reference solution (a) (Figure 0969.-1) and it does not show B. Examine the chromatograms obtained in the test for fatty enhanced peaks with retention times corresponding to cetyl alcohol and stearyl alcohol present in the chromatogram alcohols and sterols. obtained with reference solution (b). Results : the principal peaks in the chromatogram Heavy metals (2.4.8) : maximum 10 ppm. obtained with the test solution are similar in retention time and size to the principal peaks in the chromatogram 2.0 g complies with limit test C. Prepare the standard using obtained with reference solution (a). 2 ml of lead standard solution (10 ppm Pb) R. C. Dissolve 50 mg in 5 ml of methylene chloride R and Loss on drying (2.2.32) : maximum 3.0 per cent, determined add 1 ml of acetic anhydride R and 0.1 ml of sulphuric on 2.000 g by drying in an oven at 100-105 °C for 1 h. acid R. A green colour is produced. Total ash (2.4.16) : maximum 0.1 per cent, determined on 5.0 g. TESTS Melting point (2.2.15) : 45 °C to 55 °C. Allow to stand at 20 °C for 16 h. Acid value (2.5.1) : maximum 1.0, determined on 5.0 g. Hydroxyl value (2.5.3, Method A) : 140 to 180. 2708 STORAGE In a well-filled container, protected from light. See the information section on general monographs (cover pages) EUROPEAN PHARMACOPOEIA 5.0 Wool fat, hydrous Figure 0969.-1. — Chromatogram for the test for fatty alcohols and sterols (reference solution (a)) in hydrogenated wool fat 01/2005:0135 Drop point (2.2.17) : 38 °C to 44 °C, determined on the residue obtained in the test for wool-fat content. To fill the metal cup, melt the residue on a water-bath, cool to about WOOL FAT, HYDROUS 50 °C, pour into the cup and allow to stand at 15 °C to 20 °C for 24 h. Adeps lanae cum aqua Water-absorption capacity. Place 10 g of the residue obtained in the test for wool-fat content in a mortar. Add DEFINITION water R in portions of 0.2 ml to 0.5 ml from a burette, Hydrous wool fat is a mixture of 75 per cent m/m of stirring vigorously after each addition to incorporate the wool fat and 25 per cent m/m of water. It is obtained water R. The end-point is reached when visible droplets by the gradual addition of water to melted wool fat with remain which cannot be incorporated. Not less than 20 ml continuous stirring. It may contain not more than 150 ppm of water R is absorbed. of butylhydroxytoluene. Acid value (2.5.1). Not more than 0.8, determined on 5.0 g dissolved in 25 ml of the prescribed mixture of solvents. CHARACTERS Peroxide value (2.5.5). Not more than 15. A pale yellow, unctuous substance. Saponification value (2.5.6) : 67 to 79, determined on 2.00 g. IDENTIFICATION Heat under reflux for 4 h. A. In a test-tube, dissolve 0.5 g in 5 ml of chloroform R and Water-soluble oxidisable substances. To 10 ml of the add 1 ml of acetic anhydride R and 0.1 ml of sulphuric filtrate obtained in the test for water-soluble acid or alkaline acid R. A green colour develops. substances add 1 ml of dilute sulphuric acid R and 0.1 ml of B. Dissolve 50 mg in 5 ml of chloroform R, add 5 ml of 0.02 M potassium permanganate. After 10 min, the solution sulphuric acid R and shake. A red colour develops and is not completely decolourised. an intense green fluorescence appears in the lower layer. Butylhydroxytoluene. Not more than 150 ppm, determined by gas chromatography (2.2.28), using methyl decanoate R TESTS as the internal standard. Water-soluble acid or alkaline substances. Melt 6.7 g on Internal standard solution. Dissolve 0.2 g of methyl a water-bath and shake vigorously for 2 min with 75 ml of water R previously heated to 90 °C to 95 °C. Allow to cool decanoate R in carbon disulphide R and dilute to 100.0 ml and filter through filter paper previously rinsed with water R. with the same solvent. Dilute 1.0 ml of this solution to To 60 ml of the filtrate (which may not be clear) add 0.25 ml 10.0 ml with carbon disulphide R. of bromothymol blue solution R1. Not more than 0.2 ml Test solution (a). Dissolve 1.0 g of the residue obtained in of 0.02 M hydrochloric acid or 0.15 ml of 0.02 M sodium the test for wool-fat content in carbon disulphide R and hydroxide is required to change the colour of the indicator. dilute to 10.0 ml with the same solvent. General Notices (1) apply to all monographs and other texts 2709