Packaging and storage
Preserve in tight, light-resistant containers. Protect from freezing, and store at a temperature below 30
.
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).
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
Compound Name |
Approx. Relative Retention Time |
Limit (%) |
[3-[2-(Dimethylamino N-oxide)ethyl]-1H-indol-5-yl]-N-methylmethanesulfonamide |
0.3 |
0.2 |
[3-[2-(Aminoethyl)-1H-indol-5-yl]-N-methylmethanesulfonamide |
0.4 |
0.1 |
[3-[2-(Methylamino)ethyl]-1H-indol-5-yl]-N-methylmethanesulfonamide |
0.6 |
0.5 |
Sumatriptan succinate related compound C |
0.9 |
0.5 |
Sumatriptan |
1.0 |
|
Any individual unspecified impurity |
|
0.1 |
Total |
|
1.5 |
[NOTEThe calculation of total impurities includes the amount of sumatriptan related compound A, determined in the test for Limit of sumatriptan related compound A.] |
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).
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 C
14H
21N
3O
2S·C
4H
6O
4, 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.
1S (USP31)