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Xylometazoline Hydrochloride
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C16H24N2·HCl 280.84

1H-Imidazole, 2-[[4-(1,1-dimethylethyl)-2,6-dimethylphenyl]methyl]-4,5-dihydro-, monohydrochloride.
2-(4-tert-Butyl-2,6-dimethylbenzyl)-2-imidazoline monohydrochloride [1218-35-5].
» Xylometazoline Hydrochloride contains not less than 99.0 percent and not more than 101.0 percent of C16H24N2·HCl, calculated on the dried basis.
Packaging and storage— Preserve in tight, light-resistant containers.
Identification—
B: The RF value of the principal spot in the chromatogram of the Identification preparation corresponds to that of Standard preparation A as obtained in the test for Chromatographic purity.
pH 791: between 5.0 and 6.6, in a solution (1 in 20).
Loss on drying 731— Dry it at 105 for 4 hours: it loses not more than 0.5% of its weight.
Residue on ignition 281: not more than 0.1%.
Chromatographic purity—
Standard solutions— Dissolve USP Xylometazoline Hydrochloride RS in methanol, and mix to obtain Standard preparation A having a known concentration of 100 µg per mL. Dilute quantitatively with methanol to obtain Standard solutions, designated below by letter, having the following compositions:
Standard
solution		 Dilution Concentration
(µg RS per mL)		 Percentage (%,
for comparison
with test specimen)
A (undiluted) 100 0.5
B (4 in 5) 80 0.4
C (3 in 5) 60 0.3
D (2 in 5) 40 0.2
E (1 in 5) 20 0.1
Test solution— Dissolve an accurately weighed quantity of Xylometazoline Hydrochloride in methanol to obtain a solution containing 20 mg per mL.
Identification solution— Dilute a portion of the Test solution quantitatively with methanol to obtain a solution containing 100 µg per mL.
Detection reagent— Prepare (1) a solution of 0.5 g of potassium iodide in 50 mL of water, and (2) a solution of 1.5 g of soluble starch in 50 mL of boiling water. Just prior to use, mix 10 mL of each solution with 3 mL of alcohol.
Procedure— Apply separately 5 µL of the Test solution, 5 µL of the Identification solution, and 5 µL of each Standard solution to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel. Position the plate in a chromatographic chamber, and develop the chromatograms in a solvent system consisting of a mixture of methanol and ammonium hydroxide (20:1) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the plate to dry under a current of warm air for at least 30 minutes. Expose the plate to chlorine gas for not more than 5 minutes, and air-dry until the chlorine has dissipated (about 15 minutes). Spray the plate with Detection reagent, and immediately compare the intensities of any secondary spots observed in the chromatogram of the Test solution with those of the principal spots in the chromatograms of the Standard solutions: the sum of the intensities of all secondary spots obtained from the Test solution corresponds to not more than 1.0%.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Assay— Dissolve about 500 mg of Xylometazoline Hydrochloride, accurately weighed, in 70 mL of glacial acetic acid, add 10 mL of mercuric acetate TS, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically (see Titrimetry 541), using a calomel-glass electrode system. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 28.08 mg of C16H24N2·HCl.
Auxiliary Information— Staff Liaison : Kahkashan Zaidi, Ph.D., Senior Scientific Associate
Expert Committee : (AER05) Aerosols05
USP29–NF24 Page 2274
Phone Number : 1-301-816-8269