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USP 39 Official Monographs / Salicylamide 5777

1 N methanolic potassium hydroxide solution: Dis- N = normality of the sodium thiosulfate VS

solve 34 g of potassium hydroxide in sufficient metha- W = weight of Safflower Oil taken (g)
nol to produce 500 mL. Allow to settle for 24 h, and F = conversion factor, 1000 g/kg
decant the clear solution. Acceptance criteria: NMT 10.0 mEq/kg
Sample solution: Place 1 g of Safflower Oil in a small • WATER DETERMINATION, Method Ic 〈921〉: NMT 0.1%
conical flask fitted with a reflux attachment. Add 10 mL
of methanol and 0.5 mL of 1 N methanolic potassium ADDITIONAL REQUIREMENTS
hydroxide solution. Reflux the mixture for 10 min, cool, • PACKAGING AND STORAGE: Preserve in tight, light-resistant
and transfer to a separator with the aid of 15 mL of n- containers, and prevent exposure to excessive heat.
heptane. Shake with 10 mL of saturated sodium chlo- • LABELING: Label it to indicate the name and concentra-
ride solution, and allow to separate. Transfer the lower tion of any additive.
layer to another separator, and shake it with 10 mL of • USP REFERENCE STANDARDS 〈11〉
n-heptane. Wash the combined organic layers with USP Safflower Oil RS
10 mL of water, dry over anhydrous sodium sulfate, and
filter. Use a suitable portion of the filtrate.
Analysis: Inject a suitable volume into the chromato-
graph, and measure the nine main peak areas of the .

methyl esters of the fatty acids. The order of elution is Salicylamide

myristate, palmitate, stearate, oleate, linoleate, linole-
nate, arachidate, eicosenoate, and behenate.
Calculate the percentage of myristate, palmitate, stea-
rate, oleate, linoleate, linolenate, arachidate, eicose-
noate, or behenate in the portion of Safflower Oil
taken:
C7H7NO2 137.14
Result = (rU/rT) × 100 Benzamide, 2-hydroxy-;
rU = peak area of myristate, palmitate, stearate, 2-Hydroxybenzamide [65-45-2].
oleate, linoleate, linolenate, arachidate, DEFINITION
eicosenoate, or behenate Salicylamide contains NLT 98.0% and NMT 102.0% of sali-
rT = total area of the nine peaks cylamide (C7H7NO2), calculated on the anhydrous basis.
Acceptance criteria: It exhibits the composition profiles
of fatty acids shown in Table 1. IDENTIFICATION
• A. INFRARED ABSORPTION 〈197K〉
Table 1
Carbon-Chain Number of Double Percentage Delete the following:
Length Bonds (%)

USP Monographs
14 0 ≤1.0
▲ . • B. ULTRAVIOLET ABSORPTION 〈197U〉
16 0 2–10 Analytical wavelength: 302 nm
Standard solution: 16 µg/mL USP Salicylamide RS in
18 0 1–10
methanol
18 1 8–21 Sample solution: 16 µg/mL of Salicylamide in methanol
18 2 68–83 Acceptance criteria: Absorptivities, calculated on the
18 3 ≤1.5 anhydrous basis, do not differ by more than 3%.▲USP39
20 0 ≤0.5
20 1 ≤0.5 Add the following:
22 0 ≤1.0
▲ • B. The retention time of the major peak of the Sample
• FATS AND FIXED OILS, Unsaponifiable Matter 〈401〉: NMT
.

solution corresponds to that of the Standard solution, as

1.5% obtained in Assay.▲USP39
• LIMIT OF PEROXIDE
Solvent A: Chloroform and glacial acetic acid (40:60)
Potassium iodide solution: Prepare a saturated solution Delete the following:
of potassium iodide in freshly boiled and cooled water,
and store it protected from light. Discard the solution if ▲ . • C.
it gives a color on the addition of Solvent A and starch Sample solution: 20 mg/mL in alcohol
TS. Analysis: Add a few drops of ferric chloride TS to 5 mL
Sample: 10 g of Safflower Oil of Sample solution.
Analysis: Transfer the Sample to a conical flask, add Acceptance criteria: A violet color develops.▲USP39
30 mL of Solvent A, and swirl to dissolve. Add 0.5 mL of
Potassium iodide solution, and swirl the flask for 1 min, ASSAY
accurately timed. Add 30 mL of water, and titrate with
0.01 N sodium thiosulfate VS, with vigorous agitation, Change to read:
to a light yellow color. Add 0.5 mL of starch TS, and
continue the titration until the blue color has disap- • PROCEDURE
peared. Perform a blank test, and make any necessary ▲Solution A: 0.1% Formic acid in water
correction.
.

Solution B: Acetonitrile
Calculate the peroxide content, in mEq/kg, in the por- Mobile phase: See Table 1.
tion of Safflower Oil taken:
Result = [(V × N)/W] × F
V = volume of sodium thiosulfate required in the
titration (mL)

Official from May 1, 2016

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
 Accessed from 10.6.1.1 by ebsc0sa on Mon Nov 16 21:17:01 EST 2015

5778 Salicylamide / Official Monographs USP 39

Table 1 Suitability requirements

Time Solution A Solution B
Resolution: NLT 1.5 between salicylic acid related
(min) (%) (%)
compound B and salicylamide, System suitability
solution
0.0 92 8 Relative standard deviation: NMT 2.8%, Standard
6.0 55 45 solution
6.5 5 95 Analysis
8.0 5 95 Samples: Standard solution and Sample solution
8.01 92 8 Calculate the percentage of salicylic acid in the portion
12.0 92 8
of Salicylamide taken:

Diluent: Acetonitrile and water (50:50) Result = (rU/rS) × (CS/CU) × 100

System suitability solution: 1.0 mg/mL of USP Salicyla- rU = peak response of the salicylic acid peak from
mide RS and 0.001 mg/mL of USP Salicylic Acid Related the Sample solution
Compound B RS in Diluent rS = peak response of the salicylic acid peak from
Standard solution: 0.2 mg/mL of USP Salicylamide RS the Standard solution
in Diluent CS = concentration of USP Salicylic Acid RS in the
Sample solution: 0.2 mg/mL of Salicylamide in Diluent. Standard solution (mg/mL)
Pass through a suitable filter of 0.2-µm pore size. CU = concentration of Salicylamide in the Sample
Chromatographic system solution (mg/mL)
(See Chromatography 〈621〉, System Suitability.) Calculate the percentage of each unspecified impurity
Mode: LC in the portion of Salicylamide taken:
Detector: UV 300 nm
Column: 2.1-mm × 10-cm; 1.8-µm packing L1 Result = (rU/rS) × (CS/CU) × 100
Column temperature: 35°
Flow rate: 0.3 mL/min rU = peak response of each unspecified impurity
Injection volume: 1 µL from the Sample solution
System suitability rS = peak response of salicylamide from the
Samples: System suitability solution and Standard Standard solution
solution CS = concentration of USP Salicylamide RS in the
Suitability requirements Standard solution (mg/mL)
Resolution: NLT 1.5 between salicylic acid related CU = concentration of Salicylamide in the Sample
compound B and salicylamide, System suitability solution (mg/mL)
solution Acceptance criteria: See Table 2. Disregard any impu-
Relative standard deviation: NMT 0.73%, Standard rity peak less than 0.05%.
solution
Analysis
Table 2
USP Monographs

Samples: Standard solution and Sample solution

Calculate the percentage of salicylamide (C7H7NO2) in Relative Acceptance
the portion of Salicylamide taken: Retention Criteria,
Name Time NMT (%)
Result = (rU/rS) × (CS/CU) × 100 Salicylic acid related
—
compound Ba 0.93
rU = peak response from the Sample solution
.

rS = peak response from the Standard solution Salicylamide 1.00 —

CS = concentration of USP Salicylamide RS in the Salicylic acid 1.33 0.1
Standard solution (mg/mL) Individual
CU = concentration of Salicylamide in the Sample unspecified —
solution (mg/mL) impurity 0.10
Acceptance criteria: 98.0%–102.0% on the anhydrous Total impurities — 1
basis▲USP39 a. For identification only.
IMPURITIES ▲USP39
• RESIDUE ON IGNITION 〈281〉: NMT 0.1%
SPECIFIC TESTS
Delete the following:
Delete the following:
•• HEAVY METALS, Method II 〈231〉: NMT 10 ppm• (Official 1-
.

Jan-2018)
▲• MELTING RANGE OR TEMPERATURE 〈741〉: 139°–142°▲USP39
• WATER DETERMINATION, Method I 〈921〉: NMT 0.5%
.

Change to read: ADDITIONAL REQUIREMENTS

• PACKAGING AND STORAGE: Preserve in well-closed
• ORGANIC IMPURITIES containers.
▲Solution A, Solution B, Mobile phase, Diluent, Sys-
.

tem suitability solution, and Chromatographic sys-

tem: Proceed as directed in the Assay. Change to read:
Standard solution: 0.001 mg/mL each of USP Salicyla-
mide RS and USP Salicylic Acid RS in Diluent • USP REFERENCE STANDARDS 〈11〉
Sample solution: 1.0 mg/mL of Salicylamide in Diluent. USP Salicylamide RS
▲USP Salicylic Acid RS
Pass through a suitable filter of 0.2-µm pore size. .

System suitability USP Salicylic Acid Related Compound B RS

Samples: System suitability solution and Standard 4-Hydroxyisophthalic acid.
solution C8H6O5 182.13▲USP39

Official from May 1, 2016

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.