Pyrilamine Maleate
;)
1,2-Ethanediamine,N-[(4-methoxyphenyl)methyl]-N¢,N¢-dimethyl-N-2-pyridinyl-,(Z)-2-butenedioate (1:1).
2-[[2-(Dimethylamino)ethyl](p-methoxybenzyl)amino]pyridine maleate (1:1) [59-33-6].
»Pyrilamine Maleate,dried in vacuum over phosphorus pentoxide for 5hours,contains not less than 98.0percent and not more than 100.5percent of C17H23N3O·C4H4O4.
Packaging and storage—
Preserve in tight,light-resistant containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption á197Uñ—
Solution:
10µg per mL.
Medium:
0.5Nsulfuric acid.
Absorptivities at 236nm and 312nm,calculated on the dried basis,do not differ by more than 3.0%.
and 103
Loss on drying á731ñ—
Dry it in vacuum over phosphorus pentoxide for 5hours:it loses not more than 0.5%of its weight.
Residue on ignitioná281ñ:
not more than 0.1%.
Related compounds—
TEST
1—
Standard solution—
Dissolve an accurately weighed quantity of USP Pyrilamine Maleate RSin a mixture of methanol and ammonium hydroxide (200:1)to obtain a solution having a known concentration of about 0.4mg per mL.Quantitatively dilute this solution with the mixture of methanol and ammonium hydroxide (200:1)to obtain Standard solutions A,B,and Chaving the following compositions:
| Standard
solution |
Dilution | Concentration
(mg of RS per mL) |
Percentage (%, for comparison with test specimen) |
| A
B C |
(1in 4) (3in 20) (1in 20) |
0.1 0.06 0.02 |
0.5 0.3 0.1 |
Test solution—
Dissolve an accurately weighed quantity of Pyrilamine Maleate in a mixture of methanol and ammonium hydroxide (200:1)to obtain a solution having a known concentration of about 20mg per mL.
Eluant:
ethyl acetate,diethylamine,n-hexane,and methanol (93:7:1:1).
Procedure—
Apply separately 10µLof the Test solutionand 10µLof each of the three Standard solutionsto a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.[NOTE—The plate has been prewashed for 2hours with Eluant and dried.]Allow the spots on the plate to dry.Place the plate in a chromatographic chamber and develop the chromatograms in Eluantuntil 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 air-dry the plate.View the plate under short-wavelength UVlight and compare the intensities of any secondary spots from the chromatogram of the Test solutionwith those of the principal spots from the chromatograms of the Standard solutions.No secondary spot from the chromatogram of the Test solutionis larger or more intense than the principal spot from Standard solution A(0.5%),and the sum of the intensities of all secondary spots from the Test solutioncorresponds to not more than 1.0%.
TEST
2—
Mobile phase—
Prepare a filtered and degassed mixture of 0.01Mammonium acetate,methanol,and triethylamine (40:60:0.1).Make adjustments,if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard solution—
Dissolve an accurately weighed quantity of USP Pyrilamine Maleate RSin Mobile phaseto obtain a solution having a known concentration of about 0.5µg per mL.
Test solution—
Transfer about 50mg of Pyrilamine Maleate,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with Mobile phaseto volume,and mix.
Chromatographic system
(see Chromatography á621ñ)—The liquid chromatograph is equipped with a 254-nm detector and a 4.0-mm ×30-cm column that contains packing L11.The flow rate is about 1.0mLper minute.Chromatograph the Standard solution,and record the peak responses as directed for Procedure:the relative standard deviation for replicate injections is not more than 5.0%.
Procedure—
Inject a volume (about 20µL)of the Test solutioninto the chromatograph,run the chromatograph for 25minutes,record the chromatograms,and measure the peak area responses,but do not measure the maleate peak area response,which elutes near the void volume.Calculate the percentage of each impurity in the portion of pyrilamine taken by the formula:
10,000(C/W)(ri/rS),
in which Cis the concentration,in mg per mL,of USP Pyrilamine Maleate RSin the Standard solution;Wis the weight,in mg,of the Pyrilamine Maleate taken to prepare the Test solution;riis the peak area response for each impurity;and rSis the response of the Standard solution:not more than 0.3%of any individual impurity is found,and not more than 1.0%of total impurities is found.
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Assay—
Dissolve about 400mg of Pyrilamine Maleate,previously dried and accurately weighed,in 50mLof glacial acetic acid.Add 1drop of crystal violet TS,and titrate with 0.1Nperchloric acid VSto a blue-green endpoint.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 20.07mg of C17H23N3O·C4H4O4.
Auxiliary Information—
Staff Liaison:Karen A Russo,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1685
Phone Number:1-301-816-8379