Procaine Hydrochloride
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C13H20N2O2.HCl 272.78

Benzoic acid,4-amino-,2-(diethylamino)ethyl ester,monohydrochloride.
2-(Diethylamino)ethyl p-aminobenzoate monohydrochloride [51-05-8].
»Procaine Hydrochloride contains not less than 99.0percent and not more than 101.0percent of C13H20N2O2.HCl,calculated on the dried basis.
Packaging and storage— Preserve in well-closed containers.
Labeling— Where it is intended for use in preparing injectable dosage forms,the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
Identification—
A: Infrared Absorption á197Kñ.
B: Dissolve 10mg in 1mLof water,add 1drop each of hydrochloric acid and sodium nitrite solution (1in 10),then add 1mLof a solution prepared by dissolving 0.2g of 2-naphthol in 10mLof sodium hydroxide solution (1in 10),and shake:a scarlet-red precipitate is formed.
C: It responds to the tests for Chloride á191ñ.
Melting range á741ñ: between 153and 158.
Bacterial endotoxins á85ñ— Where the label states that Procaine Hydrochloride is sterile or must be subjected to further processing during the preparation of injectable dosage forms,it contains not more than 0.6USP Endotoxin Unit per mg of procaine hydrochloride.
Sterility á71ñ— Where the label states that Procaine Hydrochloride is sterile,it meets the requirements when tested as directed for Membrane Filtration under Test for Sterility of the Product to be Examined.
Acidity— To a solution of 1.0g in 25mLof water add 1drop of methyl red TS,and titrate with 0.020Nsodium hydroxide:not more than 0.50mLis required for neutralization.
Loss on drying á731ñ— Dry it over silica gel for 18hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ: not more than 0.15%.
Chromatographic purity—
Solvent— Prepare a mixture of methanol and trichloroethane (7:3).
Standard preparations— Prepare a solution of USP Procaine Hydrochloride RSin Solventcontaining 1.6mg per mL.Dilute quantitatively with Solventto obtain Standard preparations having the following compositions:
Standard
preparation		 Dilution Concentration
(mg RSper mL)		 Percentage (%,
for comparison
with test
specimen)
A 2.5in 10 0.4 0.5
B 2.0in 10 0.32 0.4
C 1.0in 10 0.16 0.2
D 0.5in 10 0.08 0.1
Test preparation— Transfer 1.6g of Procaine Hydrochloride,accurately weighed,to a suitable capped container,add 20mLof Solvent,close the container,and sonicate for 2minutes.Use this solution as the Test preparation.
Procedure— Apply separately 10µLof the Test preparationand 10µLof each Standard preparationto a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture,prewashed with methanol and allowed to dry.Use a double-trough chromatographic chamber.Fill one trough with ammonium hydroxide,and allow the chamber to equilibrate for 1hour.Position the plate in the other trough,and develop the chromatogram in a solvent system consisting of a mixture of methylene chloride and methanol (95:6)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the developing chamber,mark the solvent front,and allow the solvent to evaporate.Examine the plate under short-wavelength UVlight.Compare the intensities of any secondary spots observed in the chromatogram of the Test preparationwith those of the principal spots in the chromatograms of the Standard preparations:no secondary spot is more intense than the principal spot obtained from Standard (0.5%),and the sum of the intensities of all secondary spots obtained from the Test preparationdoes not exceed 1.0%.
Assay— Transfer about 0.5g of Procaine Hydrochloride,accurately weighed,to a beaker,add 100mLof cold water,5mLof hydrochloric acid,and 100mg of potassium bromide,and stir until dissolved.Proceed as directed under Nitrite Titration á451ñ,beginning with “cool to about 15.”Perform a blank determination,and make any necessary correction.Each mLof 0.1Msodium nitrite is equivalent to 27.28mg of C13H20N2O2.HCl.
Auxiliary Information— Staff Liaison:Karen A Russo,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1628
Pharmacopeial Forum:Volume No.29(5)Page 1565
Phone Number:1-301-816-8379