»Modified Lanolin is the purified wax-like substance from the wool of sheep,Ovis ariesLinné(Fam.Bovidae),that has been processed to reduce the contents of free lanolin alcohols and detergent and pesticide residues.It contains not more than 0.25percent of water.It may contain not more than 0.02percent of a suitable antioxidant.
Packaging and storage Preserve in tight,preferably rust-proof containers,preferably at controlled room temperature.
Acidity á401ñ The free acids in a 12.5-g portion require for neutralization not more than 2.0mLof 0.10Nsodium hydroxide.
Alkalinity Dissolve 2.5g in 10mLof ether,and add 2drops of phenolphthalein TS:no red color is produced.
Water á921ñ Dissolve about 25g,accurately weighed,in 75mLof a Mixed solventconsisting of chloroform and methanol (3:2),and dilute with Mixed solventto 100.0mL.Determine the water content of a 10-mLportion as directed under Water Determination,Method Iá921ñ.Perform a blank determination on 10mLof Mixed solvent,and make any necessary correction:not more than 0.25%is found.
Water-soluble acids and alkalies Warm 12.5g with 50mLof water on a steam bath,stirring constantly,until the lanolin is melted;the fat separates completely on cooling,leaving the water layer nearly clear and neutral to litmus.Retain the water layer for the test for Ammonia.
Ammonia Add 1mLof 1Nsodium hydroxide to a 10-mLportion of the solution from the test for Water-soluble acids and alkalies,and boil:the vapors do not turn red litmus blue.
Foreign substances Proceed as directed in the test for Foreign substancesunder Lanolin.The total limit of specified residues is not more than 3ppm with no individual specified residue exceeding 1ppm.
Limit of free lanolin alcohols
Gel permeation chromatography cleanup system
ELUANT: methylene chloride.
APPARATUS The gel permeation chromatograph is equipped with a 25-mm ×100-cm column,packed with a slurry of styrene-divinylbenzene copolymer beads compressed to a bed length of approximately 77cm.The Eluantis pumped at a flow rate of about 4mLper minute.Set up the chromatograph,adjusting to discard the fraction eluting from 0to 43minutes,collect the fraction eluting from 43to 60minutes,and rinse for 20minutes,discarding the rinse fraction.
ELUTION OF LANOLIN ALCOHOLS Melt a suitable quantity of USP Lanolin Alcohols RS,and pass through a fluted filter paper into a container.Transfer about 1.0g of warm filtered USP Lanolin Alcohols RS,accurately weighed,to a 10-mLvolumetric flask.Dilute with Eluantto volume,and mix.Transfer 5mLof this Standard solution to the gel permeation chromatographic column,and elute with Eluant.Collect 172to 240mLof the column effluent in a suitable evaporator.Evaporate the solvent,cool,weigh the evaporator,and calculate the amount of lanolin alcohols eluted in the evaporator.The column is suitable if not less than 99%of the lanolin alcohols elute in the first 172to 240mL.
Standard preparation Dissolve a suitable quantity of USP Lanolin Alcohols RS,accurately weighed,in hexane,with the aid of warming if necessary,to obtain a solution having a known concentration of about 0.5mg per mL.[NOTEStore this solution in the dark in a cold place for up to 4weeks.Before using,warm just sufficiently to dissolve any precipitate if necessary.]
Test preparation Transfer 1g of Modified Lanolin,accurately weighed and previously melted to liquid form,by heating on a hot water bath if necessary,to a 10-mLvolumetric flask,dissolve in 7mLof Eluant,dilute with Eluantto volume,mix,and filter.Transfer 5.0mLof this solution to the column,and elute with 320mLof Eluant.Discard the first 172-mLfraction,collect the next 68-mLfraction (from 172to 240mL)in a suitable evaporator.Concentrate by evaporation on a steam bath to about 3mL,add about 50mLof hexane,and transfer this solution to a 100-mLvolumetric flask,adjusting the volume with hexane to 100mL.
Chromatographic system The gas chromatograph is equipped with a flame-ionization detector maintained at 290,a 0.33-mm ×50-m fused silica capillary column bonded with a 0.50-µm layer of phase G2,a 0.32-mm ×50-cm fused silica uncoated guard column to protect the main analytical column.The column temperature is initially held at 210and programmed to rise to 280at the rate of 3per minute.Nitrogen is used as the carrier gas at a flow rate of about 7mLper minute,and is also used as the makeup gas at a flow rate of about 50mLper minute.
Procedure Separately inject equal volumes (about 1µL)of the Standard preparationand the Test preparationinto the chromatograph,and allow both the Standard preparationand the Test preparationto elute for not less than 40minutes.Record the chromatograms,and measure the areas of all of the peaks.Calculate the quantity,in percentage,of free lanolin alcohols in the portion of Modified Lanolin taken by the formula:
100(CK/IW)(rU/rS),in which rUand rSare the total peak areas found in the Test preparationand the Standard preparation,respectively;Cis the concentration,in mg per mLof USP Lanolin Alcohols RSin the Standard preparation;Iis the volume,in mL,injected into the gel permeation chromatography column;Wis the weight,in g,of Modified Lanolin taken;and Kis the corrected fraction of free lanolin alcohols in the USP Lanolin Alcohols RSin the Standard preparationtaken by the formula:
1+(0.0062A-0.0119S),in which Aand Sare the acid value and saponification value,respectively,of USP Lanolin Alcohols RS:not more than 6%is found.
Petrolatum Heat about 3g,accurately weighed,on a steam bath,with frequent stirring,until it loses about 0.25%of its weight.Boil 40mLof dehydrated alcohol with 500mg of the dried lanolin so obtained:the solution is clear or not more than opalescent.
Auxiliary Information Staff Liaison:Lawrence Evans,III,Ph.D.,Scientist
Expert Committee:(PA6)Pharmaceutical Analysis 6