Oleyl alcohol EUROPEAN PHARMACOPOEIA 5.0

— arachidic acid: not more than 2.0 per cent, Composition of fatty alcohols. Gas chromatography — eicosenoic acid:notmorethan2.0percent. (2.2.28): use the normalisation procedure. Ethylene oxide and dioxan (2.4.25). Not more than 1 ppm Test solution. Mix 25 mg of the substance to be examined of ethylene oxide and 10 ppm of dioxan. with 1.0 ml of methylene chloride R. Heavy metals (2.4.8). 2.0 g complies with limit test C for Reference solution (a). Dissolve 25 mg of each of arachidyl heavy metals (10 ppm). Prepare the standard using 2 ml of alcohol R, linolenyl alcohol R, linoleyl alcohol R, oleyl lead standard solution (10 ppm Pb) R. alcohol R, palmityl alcohol R and stearyl alcohol R in methylene chloride R and dilute to 5 ml with the same Water (2.5.12). Not more than 1.0 per cent, determined solvent. Dilute 1 ml of this solution to 5 ml with methylene on 1.0 g by the semi-micro determination of water. Use chloride R. amixtureof30volumesofanhydrous methanol R and Reference solution (b). Dissolve 10 mg of linoleyl alcohol R 70 volumes of methylene chloride R as solvent. and 1 g of oleyl alcohol R in methylenechlorideRand Total ash (2.4.16). Not more than 0.1 per cent, determined dilute to 40 ml with the same solvent. on 1.0 g. Column: STORAGE — size: l =30m,Ø=0.32mm, Store protected from light and at room temperature. — stationary phase: poly(dimethyl)siloxane R (film thickness 1 µm). LABELLING Carrier gas: helium for chromatography R. Thelabelstatesthetypeofmacrogolused(meanrelative Flow rate:1ml/min. molecular mass) or the number of units of ethylene oxide per molecule (nominal value). Split ratio:1:11. Temperature:

01/2005:2073 Time Temperature (min) (°C) OLEYL ALCOHOL Column 0-1 170 1-9 170→ 210 Alcohol oleicus 9 - 65 210 DEFINITION Injection port 270 Mixture of unsaturated and saturated long-chain fatty Detector 280 alcohols consisting mainly of octadec-9-enol (oleyl alcohol Detection:flameionisation. and elaidyl alcohol; C18H36O; Mr 268.5). It may be of vegetable or animal origin. Injection:1µl. Identify the peaks using the chromatogram obtained with CHARACTERS reference solution (a). Appearance: colourless or light yellow liquid. Relative retention with reference to oleyl alcohol (retention time = about 30 min): palmityl alcohol = about 0.6; linolenyl IDENTIFICATION alcohol = about 0.8; linoleyl alcohol = about 0.9; stearyl A.Itcomplieswiththetestforhydroxylvalue(seeTests). alcohol = about 1.1; arachidyl alcohol = about 1.9 (elaidyl B. It complies with the test for composition of fatty alcohols alcohol co-elutes with oleyl alcohol). (see Tests). System suitability: reference solution (b): TESTS — peak-to-valley ratio: minimum 1.2 between the peaks due to linoleyl alcohol and oleyl alcohol. Appearance.Thesubstancetobeexaminedisclear(2.2.1) Limits: and not more intensely coloured than reference solution B6 (2.2.2, Method II). — palmityl alcohol:maximum8.0percent, Refractive index (2.2.6): 1.458 to 1.460, determined — stearyl alcohol:maximum5.0percent, at 25 °C. — oleyl alcohol (sum of oleyl and elaidyl alcohols): Cloud point:maximum10°C. minimum 80.0 per cent, Introduce about 60 g into a cylindrical flat-bottomed — linoleyl alcohol: maximum 3.0 per cent, container, 30-33.5 mm internal diameter and 115-125 mm — linolenyl alcohol:maximum0.5percent, high. Heat to 30 °C, cool, and immerse the container in iced — arachidyl alcohol:maximum0.3percent. water with the surfaces of the water and the sample at the same level. Insert a thermometer and, using it as a stirring rod begin stirring rapidly and steadily when the temperature 01/2005:1878 falls below 20 °C. Keep the thermometer immersed throughout the test, remove and examine the container at regular intervals. The cloud point is the temperature at OLIVE LEAF which the immersed portion of the thermometer, positioned vertically in the centre of the container, is no longer visible Oleae folium when viewed horizontally through the container and sample. DEFINITION Acid value (2.5.1): maximum 1.0, determined on 5.0 g. Dried leaf of Olea europaea L. Hydroxyl value (2.5.3, Method A): 205to215. Content: minimum 5.0 per cent of oleuropein (C25H32O13 ; Saponification value (2.5.6): maximum 2.0. Mr 540.5) (dried drug).

2134 See the information section on general monographs (cover pages) EUROPEAN PHARMACOPOEIA 5.0 Olive oil, refined

CHARACTERS ASSAY Macroscopic and microscopic characters described under Liquid chromatography (2.2.29). identification tests A and B. Test solution. In a flask, place 1.000 g of the powdered drug IDENTIFICATION (355) and add 50 ml of methanol R.Heatinawater-bathat 60 °C for 30 min with shaking. Allow to cool and filter into A. The leaf is simple, thick and coriaceous, lanceolate to a 100 ml volumetric flask. Rinse the flask and the filter with obovate, 30 mm to 50 mm long and 10 mm to 15 mm methanol R anddiluteto100.0mlwiththesamesolvent. wide, with a mucronate apex and tapering at the base Dilute 2.0 ml of the solution to 20.0 ml with water R. toashortpetiole;themarginsareentireandreflexed abaxially. The upper surface is greyish-green, smooth and Reference solution. Dissolve 5.0 mg of oleuropein R in shiny, the lower surface paler and pubescent, particularly 5.0 ml of methanol R.Dilute1.0mlofthesolutionto25.0ml along the midrib and main lateral veins. with water R. B. Reduce to a powder (355). The powder is yellowish-green. Column: Examine under a microscope using chloral hydrate — size: l =0.15m,Ø=3.9mm, solution R. The powder shows the following diagnostic — stationary phase: octadecylsilyl silica gel for characters: fragments of the epidermis in surface view chromatography R (5 µm), with small, thick-walled polygonal cells and, in the — temperature:25°C. lower epidermis only, small anomocytic stomata (2.8.3); fragments of the lamina in sectional view showing a thick Mobile phase: cuticle, a palisade composed of 3 layers of cells and a — mobile phase A:dilute1.0mlofglacial acetic acid R to small-celled spongy parenchyma; numerous sclereids, 100 ml with water R, very thick-walled and mostly fibre-like with blunt or, — mobile phase B: methanol R, occasionally, forked ends, isolated or associated with Time the parenchyma of the mesophyll; abundant, very large Mobile phase A Mobile phase B peltate trichomes, with a central unicellular stalk from (min) (per cent V/V) (per cent V/V) which radiate some 10 to 30 thin-walled cells which 0-5 85→ 40 15 → 60 become free from the adjoining cells at the margin of the 5-12 40 → 20 60 → 80 shield, given an uneven, jagged appearance. 12 - 15 20 → 85 80 → 15 C. Thin-layer chromatography (2.2.27). Test solution. To 1.0 g of the powdered drug (355) add Flow rate:1ml/min. 10 ml of methanol R. Boil under a reflux condenser for Detection: spectrophotometer at 254 nm. 15 min. Cool and filter. Injection:20µl. Reference solution.Dissolve10mgofoleuropein R and Retention time:oleuropein=about9min. 1mgofrutin R in 1 ml of methanol R. Calculate the percentage content of oleuropein from the Plate: TLC silica gel plate R. expression. Mobile phase: water R, methanol R, methylene chloride R (1.5:15:85 V/V/V). Application: 10 µl as bands. Development:overapathof10cm. A area of the peak due to oleuropein in the Drying:inair. 1 = chromatogram obtained with the test solution, Detection:spraywithvanillin reagent R and heat at 100-105 °C for 5 min; examine in daylight. A2 = area of the peak due to oleuropein in the Results: see below the sequence of the zones present in chromatogram obtained with the reference the chromatograms obtained with the reference solution solution, and the test solution. Furthermore, other faint zones m1 = massofthedrugtobeexamined,ingrams, maybepresentinthechromatogramobtainedwiththe m2 = mass of oleuropein R in the reference solution, test solution. in grams, Top of the plate p = percentage content of oleuropein in oleuropein R. A dark violet-blue zone (solvent front) A dark violet-blue zone 01/2005:1456 ______

Oleuropein: a brownish-green Abrownish-greenzone OLIVE OIL, REFINED zone (oleuropein) ______Olivae oleum raffinatum Rutin: a brownish-yellow zone DEFINITION Reference solution Test solution Refined olive oil is the fatty oil obtained by refining of crude olive oil, obtained by cold expression or other suitable TESTS mechanical means from the ripe drupes of Olea europaea L. Foreign matter (2.8.2): maximum 2 per cent. A suitable antioxidant may be added. Loss on drying (2.2.32): maximum 10.0 per cent, determined CHARACTERS on 1.000 g of the powdered drug (355) by drying in an oven A clear, colourless or greenish-yellow, transparent liquid, at 100-105 °C for 2 h. practically insoluble in alcohol, miscible with light petroleum Total ash (2.4.16): maximum 9.0percent. (50°Cto70°C).

GeneralNotices(1)applytoallmonographsandothertexts 2135