1/4/2016
`
`USPMonographs PhmylephrineHydrochloride
`
`U.S. PHARMACOPEIA
`
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`Phenylephrine Hydrochloride
`
`C9H13N02HCI
`
`203.67
`
`HO
`
`H OH
`
`H
`N
`
`CH3
`
`HC!
`
`(/?)-.
`Benzenemethanol, 3-hydroxy-C(-[(methylamino)nnethyl]-, hydrochloride
`(—)-m-Hydroxy-Ct-[(methylamino)methyl]benzyl alcohol hydrochloride
`[67-76-7].
`» Phenylephrine Hydrochloride contains not less than 97.5 percent and not more than 102.5 percent of
`CgH-^NC^-HCI, calculated on the dried basis.
`
`Packaging and storage— Preserve
`30 .
`
`in
`
`tight,
`
`light-resistant containers. Store
`
`at 25°,
`
`excursions
`
`USP Reference standards ( 11.)—L/SP Phenylephrine Hydrochloride RS.
`
`Identification—
`
`A: Infrared Absorption ( 197K ).
`
`B: A solution (1 in 100) responds to
`
`the
`
`tests
`
`Meitinq range (
`
`
`
`741 ) : between 140° and 145°.
`
`Specific rotation ( 781S ) : between —42° and —47.5°.
`
`Test solution: 50 mg per mL,
`
`in
`
`water.
`
`
`
`Chloride for ( 191 ) .
`
`
`
`Loss on drying ( 731 ) — Dry it at 105°
`
`
`
`for 2 hours: it loses not more than 1.0% of its weight.
`
`Residue on ignition ( 281 ) : not more than 0.2%.
`
`
`
`
`
`in Sulfate ( 221 ) — A solution of 50 mg 25 mL of water shows no more turbidity
`
`than
`
`corresponds to
`
`
`
`0.10 mL N
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`PARAGON - EXHIBIT 2020
`
`

`
`1/4/2016
`sulfuric acid (0.20%).
`
`USPMonographs PhmylephrineHydrochloride
`
`in Limit of ketones— Dissoive 200 mg 1 mi. of water, add 2 drops of sodium nitroferricyanide TS. then add 1 mL of 1 N
`
`
`
`sodium hydroxide, foiiowed by 0.6 mL
`
`of giaciai acetic acid: the coior of the finai solution
`is
`not deeper than that
`a control solution prepared with 1 mL of dilute acetone (1 in 2000).
`
`obtained in
`
`Chromatographic purity—
`
`in
`of USP
`Standard preparations— Dissolve an accurately weighed quantity
`Phenylephrine Hydrochloride RS
`obtain a solution having a known concentration of 1 mg per mL. Quantitatively dilute with methanol to
`obtain Standard
`preparations having the
`following compositions:
`
`Standard
`Preparation Dilution
`(1 in 2)
`A
`(1 in 4)
`B
`(1 in 10)
`C
`(1 in 20)
`D
`
`Percentage (%
`Concentration for comparison
`with test
`(MO RS
`per mL)
`specimen)
`500
`1.0
`250
`0.5
`100
`0.2
`50
`0.1
`
`Test preparation— Dissolve an accurately weighed quantity of Phenylephrine Hydrochloride
`containing 50 mg per mL.
`
`in
`
`methanol
`
`to
`
`Standard each pL of to a suitable thin-layer
`
`
`preparation and 5
`the
`of
`|jL
`Procedure— Apply separately 5
`
`Test
`chromatographic plate (see Chromatoaraohv ( 621)) coated with a 0.25-mm layer of chromatographic silica
`gel mixture.
`Position the plate in a chromatographic chamber and develop
`the
`chromatograms
`in
`a
`solvent
`system
`mixture of n-butyl alcohol, water, and formic acid (7:2:1) until the solvent front has moved about three-fourths of the length
`the
`of the plate. Remove the plate
`from
`the
`developing chamber, mark
`the
`solvent
`front,
`
`and allow in
`warm, circulating air. Examine
`the plate under short-wavelength UV
`Then light. spray the plate with a saturated solution of
`
`
`p-nitrobenzenediazonium tetrafluoroborate followed by sodium
`carbonate solution
`(1
`in
`10). Compare the
`secondary spots observed in
`in
`the chromatogram of
`the
`
`preparation with those of the principal spots
`the
`Test
`chromatograms of the Standard preparations: the
`sum
`of
`the
`
`secondary of intensities spots obtained from the Test
`
`
`preparation corresponds to
`not more than 1.0% of
`related compounds, with
`
`single no corresponding to more than impurity
`
`
`0.5%.
`
`preparation
`
`Chloride content— Dissolve about 300 mg, accurately weighed, in 5 mL of water. Add 5 mL
`acetic
`glacial
`of
`mL of methanol, then add 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 CI. Not less
`
`than 17.0% and not more than 17.7% of CI is
`found, calculated on
`the
`dried basis.
`
`Residual solvents ( 467 ) : meets the requirements.
`(Official January 1, 2007)
`
`Assay— Dissolve about 100 mg of Phenylephrine Hydrochloride, accurately weighed, in 20 mL of water contained in an
`
`iodine flask, add 50.0 mL of 0.1 N bromine VS,
`add 5 then mL of hydrochloric acid, and immediately insert the stopper.
`
`
`
`Shake the flask, and allow to stand for 15 minutes. Introduce quickly
`
`10 mL of potassium iodide solution (1 in 10), allow to
`stand for 5 minutes, shake
`thoroughly, remove
`the
`
`stopper, and rinse it and the neck of the flask with a small
`quantity of
`water into the flask. Titrate the
`
`liberated iodine with 0.1 N sodium thiosulfate VS,
`adding 3 mL
`
`starch of TS as the endpoint
`
`is approached. Perform a blank determination (see Residual Titrations under Titrimetrv ( 541 )). Each mL of 0.1 N bromine
`is equivalent to 3.395 mg of C9H13NO2 HCI.
`
`Auxiliary Information— Staff Liaison : Civdewvn M. Anthonv. Ph.D.. Scientist
`
`Expert Committee :
`(MDCCA05) Monograph Development-Cough Cold and Analgesics
`USP29-NF24 Page 1712
`
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`USPMonographs PhmylephrineHydrochloride
`1/4/2016
`Volume No. 29(6) Page 1964
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