Naratriptan Hydrochloride
» Naratriptan Hydrochloride contains not less than 98.0 percent and not more than 101.0 percent of C17H25N3O2S·HCl, calculated on the anhydrous and solvent free-basis.
Packaging and storage
Preserve in tight containers, and store below 30.
USP Reference standards 11
USP Naratriptan Hydrochloride RS . USP Naratriptan Resolution Mixture RS.
noteWhen performing assays and tests, store all standard, system suitability, and sample solutions in a cool place, protected from light.
Identification
B:
The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
C:
It meets the requirements of the test for dry chlorides under Chloride 191.
Water, Method I 921:
not more than 0.5%.
Heavy metals, Method II 231:
0.002%.
Chromatographic purity
0.05 M Ammonium phosphate buffer
Dissolve 5.75 g of monobasic ammonium phosphate in 1000 mL of water, and adjust with phosphoric acid to a pH of 3.00 ± 0.05.
Solution A
Prepare a filtered and degassed mixture of 0.05 M Ammonium phosphate buffer and acetonitrile (97:3).
Solution B
Prepare a filtered and degassed mixture of 0.05 M Ammonium phosphate buffer and acetonitrile (4:1).
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).
Resolution solution
Dissolve an accurately weighed quantity of USP Naratriptan Resolution Mixture RS in water to obtain a solution having a known concentration of about 0.11 mg per mL.
Test solution
Dissolve an accurately weighed quantity of Naratriptan Hydrochloride in water to obtain a solution having a known concentration of about 0.11 mg per mL.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 225-nm detector and a 4.6-mm × 15-cm column that contains 4-µm packing L1. The column temperature is maintained at 40. The flow rate is about 1.5 mL per minute. The chromatograph is programmed as follows.
Procedure
Inject a volume (about 20 µL) of the Test solution into the chromatograph, record the chromatogram, and measure the areas for all of the peaks. Calculate the percentage of each impurity in the portion of Naratriptan Hydrochloride taken by the formula:
100(ri /F)/[rN + S(ri /F)]
in which F is the relative response factor (see the accompanying table for values) for each impurity; ri is the peak response for each impurity; and rN is the naratriptan peak response (see the accompanying table for limits).
Assay
0.01 M Triethylamine phosphate buffer
Dilute 0.6 mL of phosphoric acid with water to 900 mL, and adjust with triethylamine to a pH of 2.5.
Mobile phase
Prepare a filtered and degassed mixture of 0.01 M Triethylamine phosphate buffer and isopropyl alcohol (9:1). Make adjustments if necessary (see System Suitability under Chromatography 621).
System suitability preparation
Dissolve an accurately weighed quantity of USP Naratriptan Resolution Mixture RS in Mobile phase to obtain a solution having a concentration of about 0.7 mg per mL.
Standard preparation
Dissolve an accurately weighed quantity of USP Naratriptan Hydrochloride RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 0.11 mg per mL.
Assay preparation
Transfer about 11 mg of Naratriptan Hydrochloride, accurately weighed, to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 282-nm detector and a 4.6-mm × 15-cm column that contains 3-µm packing L11. The column temperature is maintained at 35. The flow rate is about 1.5 mL per minute. Chromatograph the System suitability preparation, and record the peak responses as directed for Procedure: the resolution, R, between naratriptan related compound A and naraptriptan and between naratriptan related compound B and naratriptan is not less than 1.5. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 1.5%. [noteFor identification purposes, the approximate relative retention times are about 0.9 for naratriptan related compound A, 1.0 for naratriptan, and 1.1 for naratriptan related compound B.]
Procedure
Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas for the major peaks. Calculate the quantity, in mg, of C17H25N3O2S·HCl in the portion of Naratriptan Hydrochloride taken by the formula:
100C(rU / rS)
in which C is the concentration, in mg per mL, of USP Naratriptan Hydrochloride RS in the Standard preparation; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
Chromatographic Column
USP32NF27 Page 3039
Pharmacopeial Forum: Volume No. 32(5) Page 1462
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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