Sumatriptan Succinate
» Sumatriptan Succinate contains not less than 98.0 percent and not more than 102.0 percent of C14H21N3O2S·C4H6O4, calculated on the solvent-free and anhydrous basis.
Packaging and storage
Preserve in tight, light-resistant containers. Protect from freezing, and store at a temperature below 30.
USP Reference standards 11
USP Sumatriptan Succinate RS. USP Sumatriptan Succinate Related Compound A RS . USP Sumatriptan Succinate Related Compound C RS . USP Sumatriptan Succinate Related Impurities RS .
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.
Water, Method I 921:
not more than 1.0%.
Limit of sumatriptan succinate related compound A
10 M Ammonium acetate solution
Dissolve 77.1 g of ammonium acetate in 100 mL of water.
Mobile phase
Prepare a filtered and degassed mixture of methanol and 10 M Ammonium acetate solution (9:1). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard solution
Dissolve an accurately weighed quantity of USP Sumatriptan Succinate Related Compound A RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 6.25 µg per mL.
Test solution
Transfer about 70 mg of Sumatriptan Succinate, accurately weighed, to a 25-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 × 25-cm column that contains 5-µm packing L3. The flow rate is about 2.0 mL per 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
Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the percentage of sumatriptan related compound A free base in the portion of sumatriptan free base taken by the formula:
100(495.7/613.8)(413.5/295.4)(CS / CU)(rU / rS)
in which 495.7 and 613.8 are the molecular weights of sumatriptan related compound A and sumatriptan succinate related compound A, respectively; 413.5 and 295.4 are the molecular weights of sumatriptan succinate and sumatriptan respectively; CS is the concentration, in mg per mL, of sumatriptan succinate related compound A in the Standard solution; CU is the concentration, in mg per mL, of sumatriptan succinate in the Test solution; and rU and rS are the peak responses of sumatriptan succinate related compound A obtained from the Test solution and the Standard solution, respectively: not more than 0.6% is found.
Related compounds
Diluent and Resolution solution
Proceed as directed in the Assay.
Buffer solution
Dissolve about 1.7 mL of dibutylamine, about 0.6 mL of phosphoric acid, and about 3.9 g of monobasic sodium phosphate dihydrate in water. Adjust with a solution of 50% (w/v) sodium hydroxide to a pH of about 7.5, dilute with water to 1000 mL, and mix.
Mobile phase
Prepare a filtered and degassed mixture of Buffer solution and acetonitrile (4:1). Make adjustments if necessary (see System Suitability under Chromatography 621).
Identification solution
Prepare a solution of USP Sumatriptan Succinate Related Impurities RS in Mobile phase having a concentration of about 3 mg per mL.
Test solution
Dissolve an accurately weighed quantity of Sumatriptan Succinate in Diluent to obtain a solution having a concentration of about 2.8 mg per mL.
Chromatographic system (see Chromatography 621)
Prepare as directed in the Assay. After making sure that the resolution criteria are met, chromatograph the Identification solution, and record the peak responses as directed for Procedure. Identify the peaks according to Table 1.
Table 1
Procedure
Inject a volume (about 10 µL) of the Test solution into the chromatograph, record the chromatogram, and measure all of the peak responses. Calculate the percentage of each impurity in the portion of Sumatriptan Succinate taken by the formula:
100(ri / rs)
in which ri is the peak response for each impurity, and rs is the sum of the responses of all the peaks: meets the requirements given in Table 1.
Assay
Diluent
Dissolve 2.97 g of monobasic sodium phosphate in 600 mL of water, adjust with a sodium hydroxide solution (1 in 2) to a pH of 6.5, dilute with water to 750 mL, add 250 mL of acetonitrile, and mix.
Mobile phase
Dissolve 1.7 mL of dibutylamine, 0.6 mL of phosphoric acid, and 3.9 g of sodium dihydrogen phosphate dihydrate in 750 mL of water, adjust with a sodium hydroxide solution (1 in 2) to a pH of 6.5, and dilute with water to 1000 mL. Mix 800 mL of this solution with 200 mL of acetonitrile, then filter and degas. Make adjustments if necessary (see System Suitability under Chromatography 621).
Resolution solution
Dissolve accurately weighed quantities of USP Sumatriptan Succinate RS and USP Sumatriptan Succinate Related Compound C RS in Diluent to obtain a solution having known concentrations of about 0.28 mg per mL and 0.14 mg per mL, respectively.
Standard preparation
Dissolve an accurately weighed quantity of USP Sumatriptan Succinate RS in Diluent to obtain a solution having a known concentration of about 0.14 mg per mL.
Assay preparation
Dissolve an accurately weighed quantity of Sumatriptan Succinate in Diluent to obtain a solution having a concentration of about 0.14 mg per mL.
Chromatographic system (see Chromatography 621)
The liquid chromatograph is equipped with a 282-nm detector and a 4.6-mm × 25-cm column that contains 5-µm packing L1. The flow rate is about 1.5 mL per minute. Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.9 for sumatriptan succinate related compound C and 1.0 for sumatriptan; and the resolution, R, between sumatriptan succinate related compound C and sumatriptan 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%.
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 of C14H21N3O2S·C4H6O4, in percentage, in the portion of Sumatriptan Succinate taken by the formula:
100(CS / CU)(rU / rS)
in which CS and CU are the concentrations, in mg per mL, of sumatriptan succinate in the Standard preparation and the Assay preparation, respectively; 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 3642
Pharmacopeial Forum: Volume No. 33(3) Page 456
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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