Hyoscyamine Sulfate Injection
» Hyoscyamine Sulfate Injection is a sterile solution of Hyoscyamine Sulfate in Water for Injection. It contains not less than 93.0 percent and not more than 107.0 percent of the labeled amount of hyoscyamine sulfate [(C17H23NO3)2·H2SO4·2H2O].
Packaging and storage Preserve in single-dose or multiple-dose containers, preferably of Type I glass, and store at controlled room temperature.
USP Reference standards 11
USP Endotoxin RS
A: 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.
B: After evaporation to dryness, or appropriate adjustment of concentration, it meets the requirements of the tests for Sulfate 191.
C: The angular rotation of the Injection is levorotatory.
Bacterial endotoxins 85 It contains not more than 714.3 USP Endotoxin Units per mg of hyoscyamine sulfate.
pH 791: between 3.0 and 6.5.
Other requirements It meets the requirements under Injections 1.
Diluent Use 0.01 N hydrochloric acid.
Buffer solution Transfer 13.6 g of monobasic potassium phosphate to a 2000-mL volumetric flask, dissolve in about 1800 mL of water, adjust with phosphoric acid to a pH of 3.0 ± 0.1, dilute with water to volume, mix, and filter.
Mobile phase With continuous stirring, add 0.3 mL of triethylamine to 1800 mL of the Buffer solution. Add 200 mL of acetonitrile, mix well, and degas.
Standard stock preparation Dissolve an accurately weighed quantity of USP Hyoscyamine Sulfate RS in Diluent to obtain a solution having a concentration of about 0.16 mg of anhydrous hyoscyamine sulfate per mL. [noteThis solution may be stored in a refrigerator for 30 days. ]
Standard preparation Transfer 3.0 mL of the Standard stock preparation into a 100-mL volumetric flask, dilute with Diluent, to volume and mix. Calculate the concentration, C, in mg per mL, of anhydrous hyoscyamine sulfate in this solution.
Assay preparation Transfer an accurately measured volume of Injection, equivalent to about 1.0 mg of hyoscyamine sulfate, to a 200-mL volumetric flask, dilute with Diluent to volume, and mix. Pass an aliquot through a 0.45-µm filter, discarding the first 5 mL of the filtrate.
Chromatographic system The liquid chromatograph is equipped with a 205-nm detector and a 4.6-mm × 15-cm column that contains 4-µm packing L11 and a 3-mm × 4-mm guard column that contains packing L11. The flow rate is about 1.0 mL per minute. The column temperature is maintained at 30. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the tailing factor is not more than 1.8, and the relative standard deviation for six replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 50 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the area responses for the major peaks. Calculate the quantity, in mg, of hyoscyamine sulfate [(C17H23NO3)2·H2SO4·2H2O] in each mL of the Injection taken by the formula:
100 × 1.053 × (C/V)(rU / rS)in which 1.053 is the ratio of the molecular weight of hydrated hyoscyamine sulfate to that of anhydrous hyoscyamine sulfate; C is as defined under Standard preparation; V is the volume, in mL, of Injection taken; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 3466Pharmacopeial Forum: Volume No. 31(5) Page 1373