HCl

1-(methylcyclopropyl)-N-(2,6-dimethylphenyl)-2-piperidinecarboxamide, hydrochloride dl-1-(methylcyclopropyl-2',6'-pipecoloxylidide, hydroxhloride.  
  
IQB-9302 hydrochloride contains not less than 98.5 percent and not more than 101.5 percent of C₁₈H₂₆N₂O.HCl calculated on the anhydrous basis. 

Packaging and storage: Preserve in well closed containers. 

Reference Standard: Use an ultrapurified lot as IQB-9302 Hydrochloride RS. 

Identification:  
A: Weigh approximately 10 mg of IQB-9302.HCl and mix with 200 mg of KBr. Using a suitable apparatus with vacuum, prepare a disk for infrared spectophotometry. The infrared spectrum of a sample of IQB-9302.HCl must exhibit the same transmittance bands that those shown  by an standard. 

B: Ultraviolet Absorption:  
Solution: 0.1 in 1000. 
Medium: distilled water. Absorptivities at 270.4 nm, calculated on the anhydrous basis, do not differ by more than 3.0%. 

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.  
Calculate the quantity of isopropanol by the  formula: 

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%. 

Chromatographic purity:  

Plates: Merck Art. 1.05735 or equivalent (5 x 10 cm) 
Eluent: methanol: ammonia (90:10) 
Solutions:  

• sample solution: dissolve 0.5 g of IQB-9302.HCl in 5 ml of methanol. >
• Reference A: dissolve 0.025 g of IQB-9302.HCl standard in 5 ml of methanol
• Reference B: dilute 0.5 ml of reference A to 100 ml with methanol (0.5%).
• Reference C: dissolve 0.25 g of aminomethylcyclopropane in 10 ml of methanol. Dilute 0.1 ml of this solution to 10 ml with methanol (0.25%).

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.