Cyclobenzaprine Hydrochloride
;)
1-Propanamine,3-(5H-dibenzo[a,d]cyclohepten-5-ylidene)-N,N-dimethyl-,hydrochloride.
N,N-Dimethyl-5H-dibenzo[a,d]cycloheptene-D5,g-propylamine hydrochloride [6202-23-9].
»Cyclobenzaprine Hydrochloride contains not less than 99.0percent and not more than 101.0percent of C20H21N·HCl,calculated on the dried basis.
Packaging and storage—
Preserve in well-closed containers.
Identification—
A:Infrared Absorption á197Mñ.
B:Ultraviolet Absorption á197Uñ—
Solution:
15µg per mL.
Medium:
methanol.
Absorptivities at 290nm,calculated on the dried basis,do not differ by more than 3.0%.
C:
Asolution (1in 50)responds to the tests for Chloride á191ñ.
Melting range á741ñ:
between 215
and 219,but the range between beginning and end of melting does not exceed 2.
and 219,but the range between beginning and end of melting does not exceed 2.
Loss on drying á731ñ—
Dry it at 105to constant weight:it loses not more than 1.0%of its weight.
to constant weight:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ:
not more than 0.1%.
Heavy metals,Method IIá231ñ:
0.001%.
Chromatographic purity—
Dissolve 100mg in methanol,and dilute with methanol to 5.0mLto obtain the Test solution.Dissolve a suitable quantity of USP Cyclobenzaprine Hydrochloride RSin methanol to obtain a Standard solutionhaving a known concentration of about 20mg per mL.Dilute a portion of this solution quantitatively and stepwise with methanol to obtain a Diluted standard solutionhaving a concentration of about 100µg per mL.Apply separate 5-µLportions of the three solutions to the starting line of a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture and previously washed with methanol.Develop the chromatogram in a suitable chamber with a freshly prepared solvent system consisting of a mixture of acetone,toluene,and ammonium hydroxide (75:25:1)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the chamber,air-dry,and view under short-wavelength UVlight:the RFvalue of the principal spot from the Test solutioncorresponds to that of the Standard solution;and any other spot obtained from the Test solutiondoes not exceed,in size or intensity,the principal spot obtained from the Diluted standard solution(0.5%).
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Test solution:
200mg per mL.
Standard solution—
Proceed as directed except to use 100.0µg of methylene chloride,12.0µg of chloroform,76.0µg of 1,4-dioxane,and 16.0µg of trichloroethylene.
Assay—
Dissolve about 400mg of Cyclobenzaprine Hydrochloride,accurately weighed,in about 80mLof glacial acetic acid,add 15mLof mercuric acetate TS,and titrate with 0.1Nperchloric acid VS,determining the endpoint potentiometrically,using a platinum ring electrode and a sleeve-type calomel electrode containing 0.1Nlithium perchlorate in glacial acetic acid (see Titrimetry á541ñ).Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 31.19mg of C20H21N·HCl.
Auxiliary Information—
Staff Liaison:Salvador C.Salado,M.S.,Scientist and Latin American Liaison
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28–NF23Page 556
Pharmacopeial Forum:Volume No.29(4)Page 1024
Phone Number:1-301-816-8165