3H-1,2,4-Triazol-3-one, 2-[3-[4-(3-chlorophenyl)-1-piperazinyl)]propyl]-5-ethyl-2,4-dihydro-4-(2-phenoxyethyl)-, monohydrochloride.
1-[3-[4-(m-Chlorophenyl)-1-piperazinyl]propyl]-3-ethyl-4-(2-phenoxyethyl)-D2-1,2,4-triazolin-5-one monohydrochloride [82752-99-6].
» Nefazodone Hydrochloride contains not less than 98.0 percent and not more than 102.0 percent of C25H32ClN5O2·HCl, calculated on the dried basis.
Packaging and storage Preserve in tight containers. Store at a temperature between 15 and 30.
USP Reference standards 11
USP Nefazodone Hydrochloride RS .
USP Nefazodone Related Compound A RS .
USP Nefazodone Related Compound B RS .
Completeness of solution 641 A 25 mg per mL solution in methanol meets the requirements.
B: A solution of 10 mg per mL meets the requirements of the test for Chloride 191.
Loss on drying 731 Dry it in vacuum at 105 for 3 hours: it loses not more than 0.5% of its weight.
Residue on ignition 281: not more than 0.1%.
Heavy metals, Method II 231: 0.001%.
Diluent Prepare a solution of water and acetonitrile (50:50).
Solution A Dissolve 0.77 g of ammonium acetate in about 950 mL of water. Adjust with triethylamine to a pH of 7.10 ± 0.05. Dilute with water to 1 L. Filter and degas.
Solution B Use filtered and degassed acetonitrile.
Mobile phase Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard stock solution Dissolve an accurately weighed amount of USP Nefazodone Hydrochloride RS in Diluent to obtain a solution containing 0.1 mg of nefazodone hydrochloride per mL.
Impurities stock solution Dissolve accurately weighed quantities of USP Nefazodone Related Compound A RS and USP Nefazodone Related Compound B RS in Diluent to obtain a final solution having a known concentration of about 0.1 mg per mL of each compound.
Resolution solution Dilute a suitable volume of the Impurities stock solution with the Standard stock solution to obtain a solution having a concentration of about 5 µg per mL each of nefazodone related compounds A and B.
Standard solution Dilute accurately measured volumes of the Impurities stock solution and the Standard stock solution quantitatively, and stepwise if necessary, with Diluent to obtain a solution having a known concentration of about 1 µg per mL each of nefazodone hydrochloride, nefazodone related compound A, and nefazodone related compound B.
Test solution Transfer about 100 mg of Nefazodone Hydrochloride, accurately weighed, to a 100-mL volumetric flask, dissolve in and dilute with Diluent to volume, and mix.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 250-nm detector and a 4.6-mm × 25-cm column that contains 5-µm packing L1. The flow rate is about 1.7 mL per minute. The chromatograph is programmed as follows.
Procedure Inject equal volumes (about 10 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the percentage of each nefazodone related compound in the portion of Nefazodone Hydrochloride taken by the formula:
100(CS /CT)(rU / rS)in which CS is the concentration, in mg per mL, of the relevant USP Reference Standard in the Standard solution; CT is the concentration of Nefazodone Hydrochloride, in mg per mL, in the Test solution; and rU and rS are the peak areas of the corresponding nefazodone related compound obtained from the Test solution and the Standard solution, respectively: not more than 0.2% of nefazodone related compound A is found; not more than 0.2% of nefazodone related compound B is found; not more than 0.1% of any unknown impurity is found; and not more than 0.5% of total impurities is found. [noteUse the peak area for nefazodone hydrochloride in the Standard solution as rS to calculate any unknown impurity.]
Assay Dissolve about 800 mg of Nefazodone Hydrochloride, accurately weighed, in 50 mL of glacial acetic acid, and add 15 mL of 3% (v/v) mercuric acetate in glacial acetic acid. Titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction (see Titrimetry 541). Each mL of 0.1 N perchloric acid VS is equivalent to 50.65 mg of C25H32ClN5O2·HCl.
Auxiliary Information Please check for your question in the FAQs before contacting USP.Chromatographic Column
USP32NF27 Page 3043Pharmacopeial Forum: Volume No. 32(5) Page 1462
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.