Nicotine Polacrilex
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» Nicotine Polacrilex is a weak carboxylic cation-exchange resin prepared from methacrylic acid and divinylbenzene, in complex with nicotine. It contains not less than 95.0 percent and not more than 115.0 percent of the labeled amount of nicotine (C10H14N2), calculated on the anhydrous basis.
Packaging and storage— Preserve in tight containers.
Identification—
A: Infrared Absorption 197K—
Test specimen— Transfer an accurately weighed quantity of Nicotine Polacrilex, equivalent to about 100 mg of nicotine, to a 100-mL glass-stoppered tube. Add 20 mL of 1 M ammonium hydroxide, 5 mL of 10 M sodium hydroxide, and 20 mL of n-hexane. Shake for 5 minutes, and allow the phases to separate. Transfer the upper hexane phase to an evaporating dish, and evaporate on a steam bath.
Standard specimen— Use USP Nicotine Bitartrate Dihydrate RS, and proceed as directed for Test specimen.
B: Infrared Absorption 197K—
Test specimen— Use the residue obtained from the Assay preparation. Decant the ammonia solution remaining in each residue, and wash the residue by shaking it with three 10-mL volumes of water, decanting the water phase after each shaking. Wash with 10 mL of 0.1 N hydrochloric acid, decant the liquid, and dry the residue at about 105.
Standard specimen— Transfer an accurately weighed portion of USP Polacrilex Resin RS, equivalent to the amount of nicotine polacrilex in the Assay preparation, to a glass-stoppered tube. Add 10 mL of 1 M ammonium hydroxide. Proceed as directed for Test specimen, beginning with “Decant the ammonia”.
Nicotine release— Transfer an accurately weighed quantity of Nicotine Polacrilex, equivalent to about 4 mg of nicotine, to a glass-stoppered test tube, add 10.0 mL of sodium chloride solution (0.9 in 100) that has been warmed to 37, and shake by mechanical means for 10 minutes. Immediately pass the liquid through a dry filter paper, discarding the first mL of the filtrate. Transfer 1.0 mL of the filtrate to a 25-mL volumetric flask, dilute with 0.1 N hydrochloric acid to volume, and mix. Determine the absorbances of the solution in a 1-cm cell at 236 nm and 282 nm and at the wavelength of maximum absorbance at about 259 nm, using 1.0 mL of sodium chloride solution (0.9 in 100) diluted to 25 mL with 0.1 N hydrochloric acid as the blank. Calculate the percentage of nicotine released by the formula:
(77400 / CW)(A259 0.5A236 0.5A282)
in which 77400 is a specific absorbance and dilution factor; C is the percentage of nicotine in the Nicotine Polacrilex on the basis of the amount determined in the Assay; W is the weight, in mg, of the Nicotine Polacrilex taken; and A259, A236, and A282 are the absorbances of the solution under test, corrected for the blank absorbances, at the wavelengths indicated by the subscripts: not less than 70% is released in 10 minutes.
Water, Method I 921— Transfer about 1.0 g of Nicotine Polacrilex, accurately weighed, to a 50-mL glass-stoppered test tube, add 20.0 mL of methanol, shake for 30 minutes, and allow to stand for about 30 minutes. Use a 10-mL portion of the methanol layer for the titration: not more than 5.0% is found.
Chromatographic purity—
Mobile phase and Chromatographic system— Proceed as directed in the Assay.
Standard solution— Transfer 1.0 mL of the Standard preparation, prepared as directed in the Assay, to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Test solution— Use the Assay preparation.
Procedure— [note—Use peak areas where peak responses are indicated.] Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, and allow the chromatograms to run for not less than two times the retention time of the major peak. Record the chromatograms, and measure the peak responses. Calculate the percentage of each impurity in the portion of Nicotine Polacrilex taken by the formula:
(162.23/462.41)(100/3)(100C / W)(ri / rS)
in which 162.23 and 462.41 are the molecular weights of nicotine and anhydrous nicotine bitartrate, respectively, C is the concentration, in mg per mL, of USP Nicotine Bitartrate Dihydrate RS on the anhydrous basis in the Standard solution, W is the weight, in mg, of nicotine in the Nicotine Polacrilex taken, and ri and rS are peak responses for the individual impurity and nicotine bitartrate dihydrate obtained from the Test solution and the Standard solution, respectively: not more than 0.3% of any individual impurity is found, and the sum of all impurities is not more than 1.0%.
Assay—
0.25 M Sodium dodecyl sulfate— Dissolve 18.02 g of sodium dodecyl sulfate in 25 mL of glacial acetic acid and sufficient water to make 250 mL, and mix.
Mobile phase— Mix 640 mL of water, 50 mL of 1 M sodium acetate, and 40 mL of 0.25 M Sodium dodecyl sulfate, and filter. Add 270 mL of acetonitrile, mix, and degas. Adjust the amount of water if necessary (see System Suitability under Chromatography 621).
Standard preparation— Dissolve an accurately weighed quantity of USP Nicotine Bitartrate Dihydrate RS in 1 M ammonium hydroxide to obtain a solution having a known concentration of about 6 mg per mL. Transfer 3.0 mL of this solution to a 10-mL volumetric flask, add 3 mL of 1 M acetic acid, dilute with water to volume, and mix.
Assay preparation— Transfer an accurately weighed quantity of Nicotine Polacrilex, equivalent to about 20 mg of nicotine, to a glass-stoppered test tube. Add 10.0 mL of 1 M ammonium hydroxide, shake for 10 minutes, and centrifuge. Transfer 3.0 mL of the clear solution to a 10-mL volumetric flask, add 3 mL of 1 M acetic acid, and dilute with water to volume. [note—Retain the resin residue from centrifugation for use in Identification test B.]
Chromatographic system (see Chromatography 621)— The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column containing packing L1. The flow rate is about 2.0 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure— Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas of the major peaks. Calculate the percentage of nicotine (C10H14N2) in the portion of Nicotine Polacrilex taken by the formula:
100(162.23 / 462.41)(100C / 3W)(rU / rS)
in which 162.23 and 462.41 are the molecular weights of nicotine and anhydrous nicotine bitartrate, respectively; C is the concentration, in mg per mL, of USP Nicotine Bitartrate Dihydrate RS on the anhydrous basis in the Standard preparation; W is the weight, in mg, of the portion of Nicotine Polacrilex taken; and rU and rS are the peak areas obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Ravi Ravichandran, Ph.D.
Senior Scientist
1-301-816-8330		 (MDPP05) Monograph Development-Psychiatrics and Psychoactives
Reference Standards Lili Wang, Technical Services Scientist
1-301-816-8129
RSTech@usp.org
USP32–NF27 Page 3081
Pharmacopeial Forum: Volume No. 28(4) Page 1168
Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.