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Salicylamide
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C7H7NO2 137.14

Benzamide, 2-hydroxy-.
2-Hydroxybenzamide [65-45-2].
» Salicylamide contains not less than 98.0 percent and not more than 102.0 percent of C7H7NO2, calculated on the anhydrous basis.
Packaging and storage— Preserve in well-closed containers.
Identification—
Solution: 16 µg per mL.
Medium: methanol.
Absorptivities at 302 nm, calculated on the anhydrous basis, do not differ by more than 3%.
C: Dissolve about 100 mg in 5 mL of alcohol, and add a few drops of ferric chloride TS: a violet color develops.
Melting range 741: between 139 and 142.
Water, Method I 921: not more than 0.5%.
Residue on ignition 281: not more than 0.1%.
Heavy metals, Method II 231: 0.001%.
Chromatographic purity—
Standard preparations— Dissolve USP Salicylamide RS quantitatively in methanol, and mix to obtain a solution having a concentration of 1.0 mg per mL. Dilute quantitatively with methanol to obtain Standard preparations, designated by letter, having the following compositions:
Standard
preparation		 Dilution Concentration
(µg RS
per mL)		 Percentage (%,
for comparison
with test
specimen)
A
B
C
D		 (1 in 5)
(3 in 20)
(1 in 10)
(1 in 20)		 200
150
100
50		 1.0
0.75
0.5
0.25
Test preparation— Dissolve 200 mg of Salicylamide in 10.0 mL of methanol, and mix.
Developing solvent system— Prepare a mixture of normal butyl acetate, chloroform, and formic acid (6:4:2).
Procedure— Apply separately 10 µL of the Test preparation and 10 µL of each of the Standard preparations to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel mixture, and dry the spots with the aid of a current of air. Place the plate in a suitable chromatographic chamber, and develop the chromatograms with the Developing solvent system 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, allow the plate to dry, and locate the spots under short-wavelength UV light. Compare the intensities of any secondary spots observed in the chromatogram of the Test preparation with those of the principal spots in the chromatograms of the Standard preparations: the total of the intensities of all secondary spots obtained from the Test preparation does not exceed that of the principal spot obtained from Standard preparation B (1%).
Organic volatile impurities, Method V 467: meets the requirements.
Solvent— Use dimethyl sulfoxide.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Assay— Transfer about 500 mg of Salicylamide, accurately weighed, to a 100-mL beaker equipped with a mechanical stirrer and a suitable cover with a single hole for the buret tip. Add 30 mL of freshly neutralized dimethylformamide containing a few drops of thymol blue TS. Titrate with 0.1 N sodium methoxide VS in toluene to the same blue endpoint obtained in the standardization of the sodium methoxide solution. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N sodium methoxide is equivalent to 13.71 mg of C7H7NO2.
Auxiliary Information— Staff Liaison : Clydewyn M. Anthony, Ph.D., Scientist
Expert Committee : (MDCCA05) Monograph Development-Cough Cold and Analgesics
USP29–NF24 Page 1939
Phone Number : 1-301-816-8139