2019 6.8 BIL sohation of prasm dityhagen Me ner Figo we 13 mixin, ‘pavcion Spectophotometer at 272 nm, Sperion 10 HL of the test solution and reference foturions (2) and (©). JRun tine 2.5 times the retention time of propyl Jpaacve retention With reference to propyl en (Getention ime = abou 4.5 min): fopucty A = about 0.3; impurity C = about 07 ‘Stem stably Reference solution (a): eohion: minimum 3,0 beeween the peaks due to impurity C and propyl parahydroxpbenzoate. = carnation foc: fo the calculation of content, peak area of impurity A by 14; — impurity A: not more than the azea of the principal peak {in the chromatogram obtained with reference solution (©) (05 per cen; — unpsced impurities: for each impity, not more than the area ofthe principal peak in the chromatogram obtained ‘with reference solution (¢) (05 per cent); — tual: not more than twice the area ofthe principal peak in the chromatogram obtained with reference solution (¢) (1.0 pet cent — diregard lic 0.2 times the area of the principal peak in ‘the chromatogram obtained with reference solution (c) (0.1 per cen) Sulfited ash (2.4.14) ‘Maximum 0.1 per cent determined on 1.0 g. ASSAY Liguid chromatography (2.2.28) as described in the tes for related substances with the following modification. Injection Test solution and reference soluson (b). CCaleulate the percentage content of CyoH,.O, from the Aecared content of propyl paraiydpbencoate CRS. IMPURITIES Speed impurities | Olher decal impurities (te follwing substances ould, if reset at a sfciet level, be detected by one or other of the tests ‘nthe monograph, The are lined bythe general acepance vt for thertenspecied impurities andor by the general monograph Sustances for pharmaceutical use (2034). It is herfore not necessary to identify thet impurities for demonsration of compliance. Sze aso 5.10. Control of impurities ‘nuances for pharmaceutical tse) B, C, D. a A. thydoxbenzsc acid, smnultipy the ° cre . B. methyl 4-hydroxybenzoate (methyl parahydcoxybenzoate), Propylene Glycol 1-725 aa . ethyl 4-hydroxybenzoate (ethyl parahydroxybenzoate), ° core Ho D. butyl 4-hydroxybenzoate (buryl parshydroxybenzoate) 2 mer Propylene Glycol (Ph. Ear. monograph 0430) , SE oy ene ne 76. CHO; Action and use ‘ Excipient. 57554 Preparation Propylene Giyeol Solution mee DEFINITION Propylene glycol is (RS)-propane-1,2-dio, (CHARACTERS A viscous, clear, colourless, hygroscopic liquid, miscible with water and with ethanol (96 per cent). IDENTIFICATION A. Relative density (Gee Tests). B. Refractive index (see Tests) C. Boiling point (2.2.12): 184 °C 10 189°C, D. To 0.5 mL add 5 mL of pyridine R and 2 g of finely ground mirobenzoyl chloride R. Boil for 1 min and pour into 15 mL of cold wazer R with shaking. Filter, wash the precipitate with 20 mL ofa saturated solution of sxion Jrydrogen carbonate R and then with water R and dry. Dissolve in boiling eshanol (80 per cmt VIV) Rand filter the hot solution. On cooling, crystals are formed which, after drying at 100-105 *C, melt (2.2.14) at 121 °C to 128 °C, ‘TESTS Appearance It is clear (2.2.1) and coloutiess (2.2.2, Method 1D, Relative density (2.2.5) 1.035 to 1.040. Refractive index (2.2.6) 1.431 to 1.433, Acidity To 10 mL add 40 mL of water R and 0.1 mL. of bromochymal ‘blue solution RI. The solution is greenish-yellow. Not more than 0.05 mi of 0.1 M sodium hydroxide is required to change the colour ofthe indicator to blue. Orxidising substances ‘To 10 mL. add 5 mL of water R, 2 mL. of pocassivm idle solution R and 2 ml. of eile sufic acid R and allow to sand in a ground-giess-stoppered flask protected from light11-726 Propylene Glycol Dicaprylocaprate 2019 for 15 min. Titrate with 0.05 M sodium shiosulars,using 1 mL. of starch solution R as indicator, Not more than 0.2 mil. 0f 0.05 M sodium thiosulfate is required, Reducing substances ‘To 1 mL add 1 mL of dius anomonia RI and heat in a water-bath at 60 °C for 5 min The sotution isnot yellow. Immediately add 0.15 mL of 0.1 M silver minaze and allow to stand for 5 min. The solution does not change its appearance Water (2.5.12) ‘Not more than 0.2 per cent, determined on 5.00 g by the semi-micro determination of water. Sulfuted ash (2.4 14) ‘Heat 50 g unt it burns and ignite. Allow to cool, Moisten the residue with sufwic acid R and ignites repeat the ‘operations. The residue weighs not more than 5 mg (0.01 per cent) STORAGE Store in an airtight container fee Propylene Glycol Dicaprylocaprate :***+ (Ph. Eur, monograph 2122) wee ‘Action and use Excpient mer DEFINITION Propylene gyol diester of saturated fay aid, msinly caprlc (octanic) sid and capric(decanci) acid, of ‘vegetable origin. CHARACTERS Appearance “Almost coloues of ight yellow, oly gud. Solubiticy Practical insoluble in wate, soluble infty ois and in ight ‘petroleum, slightly soluble in anhydrous ethanol. IDENTIFICATION First identification: C, D. Second identification: A, B, C, E, A. Reactive index (2.26): 1.439 to 1.442. B. Relative density (2.2.5): 0.910 to 0.930, C. Viscoscy (2.2.91: 9 mPa to 13 mPa D. Composition off aids (ce Test). E, Suponiicaton value (see Tess). TESTS Appearance ‘The substance to be examined is clear (2.2.1) and not more intensely coloured than reference solution BYe (2.22, ‘Mathad 1), Acid value (25.1) Maximum 02. Hydroxyl value (2.5.3, Mathod A) Maximum 10 Todine value (2.54 ‘Masxmam 1.0 Peroxide value (25.5, Maiod A) Maximum 1.9. Saponification value (2.5.6) 313 1 340. ‘Alkaline impurities Dissolve 2.00 g ofthe substance tobe examined in a £15 ml of ethana (96 por con) Rand 3.0 mL of es ‘Ad 0.05 ml. of bromophenol blue soluion R. Not more i 2.15 ml of 0.01 M hha acids raed to chang colour ofthe indicator to yellow. Composition of fatty acids Gas chromatography (2.422, Meta C). Prepare reference solution (a as indicated in Table 2.4222 Column: ‘ = materia ase sites — size: 1= 30 m, © = 0.32 mam; — stationary phase: mace! 20 000 (fim thickness 05 wn). Carter gat halon for chromaograpy R. Flo rae 13 mien ‘Split rato 12100, Temperanure: Sime Femapernase (oxi) co) Coane rr tess 70+ 240 35-50 20 ejection por 250 Dazcoe 230 Datsction Flame ionisation Composition of the fatry-acd fraction of the substance = caproie acid: maxizaum 2.0 per cent — aprile acide 50.0 per cent to 80.0 per cents capric acid: 20.0 pee cent to 50.0 per cent; — laurie acid: maxienum 3.0 per cent; — myristic acid: maximum 1.0 per cent. Water (2.5.12) ‘Maximum 0.1 per cent, determined on 5.00 g. Total ash (2.4.16) ‘Maximum 0.1 per cent, determined.on 2.0 g, STORAGE Protected from light. Propylene Glycol Dilaurate ? "5 Pk, Be. monograph 2087) oe Action and use Bipient mer _ DEFINITION ‘Mixture of propylene glycol (2RS)-propane-1,2-diol) mono- and diesters of laurie (dodecanoie) acid. Content ‘Minimum 70.0 per cent of dieaters and maximum 30.0 per cent of manoesters CHARACTERS Appearance Clear, oily liquid at 20 °C, colourless or slightly yellow.