Calcium Undecylenate
»Calcium Undecylenate contains not less than 98.0percent and not more than 102.0percent of C22H38O4Ca (calcium undecylenate),calculated on the dried basis.
Packaging and storage
Preserve in well-closed containers.
Identification
A:
Afiltered solution (1in 20)in 3Nhydrochloric acid responds to the tests for Calcium á191ñ.
B:
Transfer 40mLof water and 10g of calcium undecylenate to a 250-mLseparator.Cautiously and slowly add 10mLof hydrochloric acid,while swirling.Insert the stopper,and shake.[NOTEThe separator will become quite warm,and pressure must be carefully and frequently relieved through the stopcock.If a curdy,white material remains after 5minutes of shaking,add additional hydrochloric acid,1mLat a time,and shake until a clear oily phase is formed.]Allow the phases to separate,drain,and discard the bottom aqueous layer.Drain and discard the middle oily layer,if present.Filter the top layer of undecylenic acid through a pledget of cotton into a 10-mLgraduated cylinder,noting the volume obtained.Transfer the filtrate to a 250-mLflask,and add an equal volume of aniline.Reflux for 1hour,swirling the flask occasionally.Allow to cool,and pour 60mLof alcohol through the condenser into the flask.Remove the flask from the condenser,add 1g of charcoal,and stir.Filter the slurry into a 250-mLbeaker.Add water dropwise until a few crystals form or the solution becomes slightly cloudy.[NOTEIf too much water is added,an oil will form.Add alcohol dropwise until the oil dissolves.]Allow the mixture to stand or refrigerate until crystals are formed.Collect the crystals on a filter paper inserted in a 45-mm porous glass filter funnel.Wash the crystals with 75mLof 25%alcohol:the crystals have a clean,white,glossy appearance.If not,recrystallize by dissolving the crystals in about 50mLof alcohol.Add about 1g of charcoal,stir,filter into a 150-mLbeaker,and continue as directed above,beginning with Add water dropwise.Dry the crystals in vacuum at 50for 2hours:the crystals so obtained melt between 66and 67.5,the procedure for Class Iabeing used (see Melting Range or Temperature á741ñ).[NOTEIf the melting point is low,additional drying or recrystallization may be necessary.]
Loss on drying á731ñ
Dry it at 105for 2hours:it loses between 2.0%and 5.7%of its weight.
Particle size,Method Iá786ñ
Test in accordance with this procedure,except to use not more than 25g,and except that a single No.100sieve is used and is to be shaken for not less than 30minutes or until sifting is practically complete:not less than 99.0%of it passes through a No.100sieve.
Limit of free undecylenic acid
Transfer 10g of Calcium Undecylenate,accurately weighed,to a 400-mLbeaker,add 250mLof solvent hexane,and mix for 2hours using a magnetic stirrer.Filter into a 500-mLflask,evaporate with the aid of a current of air to about 20mL,and add 100mLof neutralized alcohol.Add 3drops of phenolphthalein TS,and titrate with 0.1Nsodium hydroxide VS.Each mLof 0.1Nsodium hydroxide is equivalent to 18.43mg of C11H20O2:not more than 0.1%is found.
Assay
Boil 40.0mLof 0.1Nhydrochloric acid VSwith about 600mg of Calcium Undecylenate,accurately weighed,for 10minutes,or until the undecylenic acid layer is clear,adding water,as necessary,to maintain the original volume.Transfer the mixture,with the aid of water,to a 500-mLseparator.Dilute with water to about 75mL,and extract with two 100-mLportions of solvent hexane.Wash the combined extracts with water until the last washing is neutral to litmus,add the washings to the original water layer.Cool,add 3drops of methyl orange TS,and titrate the excess hydrochloric acid with 0.1Nsodium hydroxide VS.Perform a blank determination (see Residual Titrationsunder Titrimetry á541ñ).Each mLof 0.1Nsodium hydroxide is equivalent to 20.33mg of C22H38O4Ca.
Auxiliary Information
Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28NF23Page 334
Phone Number:1-301-816-8394
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