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Propyl parahydroxybenzoate

EUROPEAN PHARMACOPOEIA 5.0

Loss on drying (2.2.32). Not more than 0.5 per cent, determined on 1.000 g by drying in an oven at 100-105 °C. Sulphated ash (2.4.14). Not more than 0.1 per cent, determined on 1.0 g. ASSAY Dissolve 0.100 g in methanol R and dilute to 250.0 ml with the same solvent. Dilute 5.0 ml of the solution to 200.0 ml with methanol R. Measure the absorbance (2.2.25) at the absorption maximum at 275 nm. Calculate the content of C10H12O5 taking the specific absorbance to be 503.

sodium carbonate solution R ; the substance partly dissolves (solution B). Add at the same time to solution A and solution B 5 ml of aminopyrazolone solution R and 1 ml of potassium ferricyanide solution R and mix. Solution B is yellow to orange-brown. Solution A is orange to red, the colour being clearly more intense than any similar colour which may be obtained with solution B.

TESTS Solution S. Dissolve 1.0 g in alcohol R and dilute to 10 ml with the same solvent. Appearance of solution. Solution S is clear (2.2.1) and not more intensely coloured than reference solution BY6 (2.2.2, STORAGE Method II). Protected from light. Acidity. To 2 ml of solution S add 3 ml of alcohol R, 5 ml of carbon dioxide-free water R and 0.1 ml of bromocresol IMPURITIES green solution R. Not more than 0.1 ml of 0.1 M sodium Specified impurities : A. hydroxide is required to change the colour of the indicator to blue. Related substances. Thin-layer chromatography (2.2.27). Test solution (a). Dissolve 0.10 g of the substance to be examined in acetone R and dilute to 10 ml with the same solvent. Test solution (b). Dilute 1 ml of test solution (a) to 10 ml A. 3,4,5-trihydroxybenzoic acid (gallic acid). with acetone R. Reference solution (a). Dilute 0.5 ml of test solution (a) to 01/2005:0431 100 ml with acetone R. Reference solution (b). Dissolve 10 mg of propyl parahydroxybenzoate PROPYL PARAHYDROXYBENZOATE with the same solvent. CRS in acetone R and dilute to 10 ml Reference solution (c). Dissolve 10 mg of ethyl Propylis parahydroxybenzoas parahydroxybenzoate CRS in 1 ml of test solution (a) and dilute to 10 ml with acetone R. Plate : suitable octadecylsilyl silica gel with a fluorescent indicator having an optimal intensity at 254 nm as the coating substance. Mobile phase : glacial acetic acid R, water R, methanol R (1:30:70 V/V/V). C10H12O3 Mr 180.2 Application : 2 µl. DEFINITION Development : over a path of 15 cm. Propyl 4-hydroxybenzoate. Drying : in air. Content : 98.0 per cent to 102.0 per cent. Detection : examine in ultraviolet light at 254 nm. System suitability : the chromatogram obtained with CHARACTERS reference solution (c) shows 2 clearly separated principal Appearance : white, crystalline powder. spots. Solubility : very slightly soluble in water, freely soluble in Limits : alcohol and in methanol. — any impurity : any spot in the chromatogram obtained IDENTIFICATION with test solution (a), apart from the principal spot, is not more intense than the spot in the chromatogram obtained First identification : A, B. with reference solution (a) (0.5 per cent). Second identification : A, C, D. Sulphated ash (2.4.14) : maximum 0.1 per cent, determined A. Melting point (2.2.14) : 96 °C to 99 °C. on 1.0 g. B. Infrared absorption spectrophotometry (2.2.24). Comparison : propyl parahydroxybenzoate CRS. ASSAY C. Examine the chromatograms obtained in the test for To 1.000 g add 20.0 ml of 1 M sodium hydroxide. Heat at related substances. about 70 °C for 1 h. Cool rapidly in an ice bath. Prepare a Results : the principal spot in the chromatogram obtained blank in the same manner. Carry out the titration on the solutions at room temperature. Titrate the excess sodium with test solution (b) is similar in position and size to hydroxide with 0.5 M sulphuric acid, continuing the titration the principal spot in the chromatogram obtained with until the second point of inflexion and determining the reference solution (b). end-point potentiometrically (2.2.20). D. To about 10 mg in a test-tube add 1 ml of sodium carbonate solution R, boil for 30 s and cool (solution A). 1 ml of 1 M sodium hydroxide is equivalent to 180.2 mg of To a further 10 mg in a similar test-tube add 1 ml of C10H12O3. 2326 See the information section on general monographs (cover pages)

Add 0. Heat 50 g until it burns and ignite. of vegetable origin.01 M hydrochloric acid is required to change the colour of the indicator to yellow.2 per cent. Refractive index (2.2.05 ml of bromophenol blue solution R. 12 ml of the solution complies with limit test A for heavy metals (5 ppm m/V).4. The substance to be examined is clear (2.2. To 1 ml add 1 ml of dilute ammonia R1 and heat in a water-bath at 60 °C for 5 min. Boil for 1 min and pour into 15 ml of cold water R with shaking.00 g of the substance to be examined in a mixture of 1.5. Immediately add 0.8).1 PROPYLENE GLYCOL DICAPRYLOCAPRATE Propylenglycoli dicaprylocapras DEFINITION CHARACTERS Propylene glycol diesters of saturated fatty acids.5.910 to 0. Hydroxyl value (2.6) : 1. The solution does not change its appearance.5 ml of ethanol (96 per cent) R and 3.433.0.4. Method A) : maximum 10. B. TESTS Appearance. Dissolve in boiling ethanol (80 per cent V/V) R and filter the hot solution.442.2.5. Water (2.EUROPEAN PHARMACOPOEIA 5.930. To 10 ml add 40 ml of water R and 0.1) and colourless (2. after drying at 100-105 °C.2. Not more than 0.2.2. Sulphated ash (2.2. It complies with the test for composition of fatty acids (see Tests). melt (2. It is clear (2.2. Viscosity (2. oily liquid.0 Propylene glycol dicaprylocaprate IMPURITIES A.3.1) and not more intensely coloured than reference solution BY6 (2. The residue weighs not more than 5 mg (0.439 to 1.0 ml of ether R. D. The solution is greenish-yellow.5) : 1. Method II). Alkaline impurities.0 g.6) : 320 to 340. D. miscible with caprylic acid (octanoic acid . 01/2005:0430 Reducing substances.1) : maximum 0. Relative density (2. R = H : 4-hydroxybenzoic acid. Saponification value (2.2 ml of 0.15 ml of 0.00 g by the semi-micro determination of water. Acidity.05 ml of 0.5.12) : 184 °C to 189 °C.2.2. Acid value (2. B. Heavy metals (2. Relative density (2. Method A) : maximum 1.5. IDENTIFICATION A. TESTS Appearance. Method II).15 ml of 0. wash the precipitate with 20 ml of a saturated solution of sodium hydrogen carbonate R and then with water R and dry. Allow to cool.1 M silver nitrate and allow to stand for 5 min.3 per cent. It complies with the test for refractive index (see Tests).4) : maximum 1.9) : 9 mPa·s to 12 mPa·s. Iodine value (2.2. C8H16O2) and capric acid (decanoic acid . Not more than 0. water and with ethanol (96 per cent). Oxidising substances.431 to 1.1 M sodium hydroxide is required to change the colour of the indicator to blue.5. using 1 ml of starch solution R as indicator.0. C. It complies with the test for relative density (see Tests). Unsaponifiable matter (2. determined on 5.5. STORAGE Store in an airtight container. PROPYLENE GLYCOL Propylenglycolum 01/2005:2122 C 3 H 8 O2 DEFINITION Propylene glycol is (RS)-propane-1.14) at 121 °C to 128 °C. 2327 . C. C.2-diol. R = CH2-CH3 : ethyl 4-hydroxybenzoate. R = CH3 : methyl 4-hydroxybenzoate. soluble in fatty oils and in light petroleum.7) : maximum 0. repeat the operations. Moisten the residue with sulphuric acid R and ignite .05 M sodium thiosulphate is required. crystals are formed which. Boiling point (2.2.14). determined on 5. slightly soluble in anhydrous ethanol. Titrate with 0. Not more than 0. clear. hygroscopic liquid. Filter.01 per cent). D. Prepare the reference solution using lead standard solution (1 ppm Pb) R. 2 ml of potassium iodide solution R and 2 ml of dilute sulphuric acid R and allow to stand in a ground-glass-stoppered flask protected from light for 15 min. R = CH2-CH2-CH2-CH3 : butyl 4-hydroxybenzoate. Mr 76. Solubility : practically insoluble in water.6) : 1. Refractive index (2. To 10 ml add 5 ml of water R. B.5. Mix 4 ml with 16 ml of water R.5 ml add 5 ml of pyridine R and 2 g of finely ground nitrobenzoyl chloride R. Dissolve 2.1 ml of bromothymol blue solution R1. Not more than 0.5) : 0.12). Peroxide value (2. IDENTIFICATION A. C10H20O2).2. On cooling. The solution is not yellow.040. General Notices (1) apply to all monographs and other texts CHARACTERS Appearance : almost colourless to light yellow. colourless.05 M sodium thiosulphate.2.035 to 1. mainly A viscous. To 0.