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Tubocuraranium, 7¢,12¢-dihydroxy-6,6¢-dimethoxy-2,2¢,2¢-trimethylchloride, hydrochloride, pentahydrate.
(+)-Tubocurarine chloride hydrochloride pentahydrate [6989-98-6].
Anhydrous 681.66 [57-94-3].
» Tubocurarine Chloride contains not less than 95.0 percent and not more than 105.0 percent of C37H41ClN2O6·HCl, calculated on the anhydrous basis.
Packaging and storage Preserve in tight containers.
USP Reference standards 11
Clarity of alcohol solution A solution of 100 mg in 10 mL of alcohol is clear.
B: The chromatogram of the Assay preparation obtained as directed in the Assay exhibits a major peak, the retention time of which corresponds to that exhibited in the chromatogram of the Standard preparation.
C: A solution (1 in 100) responds to the tests for Chloride 191.
Specific rotation 781S: between +210 and +224.
Test solution: 10 mg per mL, in water, allowed to stand for 3 hours.
Water, Method I 921: not more than 12.0%.
Residue on ignition 281: not more than 0.25%.
Related compounds In the chromatogram obtained from the Assay preparation in the Assay, the sum of the responses of any peaks detected, other than the peak due to tubocurarine, is not more than 5.0% of the total of all peak responses.
Chloride content Dissolve about 300 mg, accurately weighed, in 5 mL of water, warming slightly to effect solution. Add 5 mL of glacial acetic acid and 50 mL of methanol, and cool to room temperature. Add 1 drop of eosin Y TS, and titrate with 0.1 N silver nitrate VS. Each mL of 0.1 N silver nitrate is equivalent to 3.545 mg of Cl. Not less than 9.9% and not more than 10.7% of Cl is found, calculated on the anhydrous basis.
Mobile phase Mix 3 volumes of acetonitrile and 2 volumes of methanol, and allow the mixture to attain room temperature. To 270 mL of this solution in a 1-liter graduated cylinder add 20.0 mL of 25% tetramethylammonium hydroxide solution in methanol, and add water to make 1 L. Adjust with phosphoric acid to a pH of 4.0, filter, and degas.
Standard preparation Dissolve an accurately weighed quantity of USP Tubocurarine Chloride RS in Mobile phase to obtain a solution having a known concentration of about 0.3 mg per mL.
Assay preparation Transfer 30 mg of Tubocurarine Chloride, accurately weighed, to a 100-mL volumetric flask. Dissolve in Mobile phase, dilute with Mobile phase to volume, and mix.
System suitability preparation Dissolve suitable quantities of tubocurarine chloride and phenol in Mobile phase to obtain a solution containing about 0.30 mg and 0.50 mg per mL, respectively.
Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 220-nm detector, and a 4-mm × 25-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the System suitability preparation, and record the peak responses as directed for Procedure: the resolution, R, between the two major peaks is not less than 2.0, and the tailing factor, T, for tubocurarine chloride is not more than 2.0. The relative standard deviation for replicate injections of the Standard preparation is not more than 2.0%. The relative retention times are about 0.50 and 1.0 for tubocurarine chloride and phenol, respectively.
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 responses for the major peaks. Calculate the quantity, in mg, of C37H41ClN2O6·HCl in the portion of Tubocurarine Chloride taken by the formula:
100C(rU / rS)in which C is the concentration, in mg per mL, of USP Tubocurarine Chloride RS in the Standard preparation, and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 4971Pharmacopeial Forum: Volume No. 29(6) Page 1996