![]() 1-(methylcyclopropyl)-N-(2,6-dimethylphenyl)-2-piperidinecarboxamide,
hydrochloride dl-1-(methylcyclopropyl-2',6'-pipecoloxylidide, hydroxhloride.
Packaging and storage: Preserve in well closed containers. Reference Standard: Use an ultrapurified lot as IQB-9302 Hydrochloride RS. Identification:
B: Ultraviolet Absorption:
C: Dissolve about 50 mg in 10 mL of water in a small separator, render alkaline with 6 N ammonium hydroxide, and extract with 10 mL of ether: the aqueous layer responds to the for Chloride. pH: between 4.5 and 6.0, in a solution (1 in 100). Loss on drying: max 1%. Residue on ignition: not more than 0. 1 %. Heavy metals: Method II: not more than 10 ppm. Residual isopropanol. Isopropanol standard solution- Pipet 0.1 mL of isopropanol into a 50-mL volumetric flask, dilute with water to volume, and mix (Solution A). Transfer 5.0 mL of this solution to a 100-mL volumetric flask, dilute with water to volume, and mix. Test preparation- Transfer 1.0 g of IQB-9302 Hydrochloride accurately weighed, to a 10-mL volumetric flask, dilute with water to volume, and mix. Chromatographic system- Under typical conditions, the instrument is equipped with a flame-ionization detector and contains a 2-m X 6-mm column containing packing S3. The injection port is maintained at a temperature of about 200º C , the column at about 175º C, the detector at about 280º C , and nitrogen is used as the carrier gas at a flow rate of about 40 mL per minute. Procedure- Inject equal volumes
(about 5 mL) of
the Test Preparation, and the Isopropyl Standard solution successively
into the gas chromatograph. Measure the responses of the alcohol peak and
the isopropyl alcohol peak in each chromatogram.
ppm isopropanol = (Am/Ap) x 1000 in which Am and Ap are the peak areas of sample and standard respectively. The content of isopropyl alcohol must not exceed 0.5%. Plates: Merck Art. 1.05735
or equivalent (5 x 10 cm)
Any secondary spot in sample solution is not more intense than the spot obtained with reference C. Assay: Transfer about 200 mg of IQB-9302.HCl, accurately weighed, to a 250-mL conical flask, and dissolve in 40 mL of glacial acetic acid. Add 10 mL of mercuric acetate TS and titrate with 0.1 N perchloric acid VS potentiometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 32.28 mg of C18H26N2O.HCl. |