(hye'' oh sye' a meen sul' fate).
Benzeneacetic acid, -(hydroxymethyl)-, 8-methyl-8-azabicyclo[3.2.1]oct-3-yl ester, [3(S)-endo]-, sulfate (2:1), dihydrate.
1h,5h-Tropan-3-ol ()-tropate (ester) sulfate (2:1) (salt) dihydrate [6835-16-1].
Anhydrous 676.83 [620-61-1].
» Hyoscyamine Sulfate contains not less than 98.5 percent and not more than 100.5 percent of (C17H23NO3)2·H2SO4, calculated on the anhydrous basis. [CautionHandle Hyoscyamine Sulfate with exceptional care, since it is highly potent. ]
Packaging and storage Preserve in tight, light-resistant containers.
USP Reference standards 11
B: The retention time of the major peak in the chromatogram of the Test solution corresponds to that in the chromatogram of the Standard solution, as obtained in the test for Chromatographic purity.
C: A solution (1 in 20) responds to the tests for Sulfate 191.
Specific rotation 781S: between 24 and 29, measured at 20.
Test solution: 50 mg per mL, in water.
Water, Method Ia 921: between 2.0% and 5.5%.
Residue on ignition 281: not more than 0.1%.
Buffer solution Dissolve 7.0 g of monobasic potassium phosphate in 1000 mL of water, adjust with 0.05 M phosphoric acid to a pH of 3.3, and mix.
Solution A Dissolve 3.5 g of sodium dodecyl sulfate in 606 mL of Buffer solution, add 320 mL of acetonitrile, and mix.
Solution B Use 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 quantity of USP Hyoscyamine Sulfate RS in Solution A to obtain a solution having a known concentration of about 1.2 mg of hyoscyamine sulfate per mL.
Standard solution Dilute a portion of the Standard stock solution with Solution A to obtain a solution having a known concentration of about 0.24 mg of hyoscyamine sulfate per mL.
Diluted standard solution Dilute the Standard solution with Solution A to obtain a solution having a known concentration of about 0.24 µg of hyoscyamine sulfate per mL.
System suitability solution Prepare a solution of USP Hyoscyamine Related Compound A RS in Solution A having a concentration of about 2.4 µg per mL. Transfer 5.0 mL of this solution to a 50-mL volumetric flask, add 10 mL of the Standard stock solution, dilute with Solution A to volume and mix.
Test solution Transfer about 60 mg of Hyoscyamine Sulfate, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Solution A to volume, and mix. Transfer 10 mL of this solution to a 50-mL volumetric flask, and dilute with Solution A to volume. This solution contains about 0.24 mg of hyoscyamine sulfate per mL.
Chromatographic system (see Chromatography 621 The liquid chromatograph is equipped with a 210-nm detector and a 4.6-mm ×10-cm column that contains 3-µm packing L1. The flow rate is about 1.0 mL per minute. The chromatograph is programmed as follows.
Procedure Separately inject equal volumes (about 10 µL) of the Diluted standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses of the major peaks. Calculate the percentage of each impurity in the portion of Hyoscyamine Sulfate taken by the formula:
0.1(CS / CT) (ri / rS)in which CS is the concentration, in µg per mL, of hyoscyamine sulfate in the Diluted standard solution; CT is the concentration, in mg per mL, of hyoscyamine sulfate in the Test solution; ri is the peak response for each impurity obtained from the Test solution; and rS is the hyoscyamine peak response obtained from the Diluted standard solution. In addition to not exceeding the limits for each impurity in Table 1, not more than 0.1% of any other individual impurity is found; and not more than 0.5% of total impurities is found.
Assay Dissolve about 0.5 g of Hyoscyamine Sulfate, accurately weighed, in 50 mL of glacial acetic acid, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 67.68 mg of (C17H23NO3)2·H2SO4.
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USP35NF30 Page 3464Pharmacopeial Forum: Volume No. 33(4) Page 659