Interim Revision AnnouncementOfficial January 1, 2017 Aspirin 1

. Acceptance criteria: 90.0%–110.0%Aspirin Boluses PERFORMANCE TESTS

DEFINITIONChange to read:Aspirin Boluses contain NLT 90.0% and NMT 110.0% of

the labeled amount of aspirin (C9H8O4).• DISSOLUTION ⟨711⟩

IDENTIFICATION Medium: 0.5 M phosphate buffer (see Reagents, In-• A. PROCEDURE dicators, and Solutions—Buffer Solutions), pH 7.4;

Analysis: Crush 1 Bolus. Boil a portion of the powder, 900 mLequivalent to 300 mg of aspirin, with 50 mL of water. Apparatus 2: 75 rpmCool and add a drop of ferric chloride TS. Time: 45 min

Acceptance criteria: A violet-red color is produced. Diluent: Acetonitrile and formic acid (99:1)• B. The retention time of the aspirin peak of the Sample Standard solution: USP Aspirin RS in •.Diluent• (IRA 1-Jan-

solution corresponds to that of the Standard solution, as 2017) at a suitable concentration. [NOTE—Prepare the so-obtained in the Assay. lution at the time of use.]

Sample solution: Pass a portion of the solution underASSAY test through a suitable filter. Dilute with Diluent, if

necessary.Instrumental conditionsChange to read:Mode: UV-VisAnalytical wavelength: The isosbestic point of aspirin• PROCEDUREand salicylic acid at 265 ± 2 nmMobile phase: 2 g/L of sodium 1-heptanesulfonate in

Analysisa mixture of acetonitrile and water (15:85). Adjust withSamples: Standard solution and Sample solutionglacial acetic acid to a pH of 3.4. •

.Calculate the percentage of the labeled amount ofDiluent: Acetonitrile and formic acid (99:1)aspirin (C9H8O4) dissolved:Standard solution: 0.4 mg/mL of USP Aspirin RS and

0.01 mg/mL of USP Salicylic Acid RS in Diluent Result = (AU/AS) × CS × V × D × (1/L) × 100•.Sample stock solution: Nominally 4 mg/mL of aspi-rin prepared as follows. Finely powder NLT 10 Boluses. AU = absorbance of the Sample solutionTransfer a portion of the powder to an appropriate vol- AS = absorbance of the Standard solutionumetric flask and dilute with Diluent to volume. Stir the CS = concentration of the Standard solutionsolution by mechanical means for 15 min. (mg/mL)Sample solution: Nominally 0.4 mg/mL of aspirin from V = volume of Medium, 900 mLSample stock solution in Diluent. Pass a portion of this D = dilution factor of the Sample solution, ifsolution through a filter of 0.5-µm or finer pore size. necessaryUse the filtrate.• (IRA 1-Jan-2017) L = label claim (mg/Bolus)• (IRA 1-Jan-2017)Chromatographic system Tolerances: NLT 80% (Q) of the labeled amount of(See Chromatography ⟨621⟩, System Suitability.) aspirin (C9H8O4) is dissolved.Mode: LC • UNIFORMITY OF DOSAGE UNITS ⟨905⟩: Meet theDetector: UV 254 nm requirementsColumn: 4.6-mm × 25-cm; 5-µm packing L1Flow rate: 1 mL/min IMPURITIESInjection volume: 20 µL

System suitabilityChange to read:Sample: Standard solution

[NOTE—The relative retention times for salicylic acid• LIMIT OF SALICYLIC ACIDand aspirin are 0.6 and 1.0, respectively.]

Mobile phase, Diluent, •.• (IRA 1-Jan-2017) Sample solution,Suitability requirementsChromatographic system, and System suitability:•

.Resolution: NLT 2.0 between salicylic acid and as-Proceed as directed in the Assay.pirin• (IRA 1-Jan-2017) •

.Salicylic acid standard solution: 0.01 mg/mL of USPRelative standard deviation: NMT 2.0% for aspirinSalicylic Acid RS in Diluent• (IRA 1-Jan-2017)Analysis

AnalysisSamples: Standard solution and Sample solutionSamples: Sample solution and •.Salicylic acid standard•

.Calculate the percentage of the labeled amount ofsolution• (IRA 1-Jan-2017)aspirin (C9H8O4) in the portion of Boluses taken:

Calculate the actual concentration (C), in mg/mL, ofResult = (rU/rS) × (CS/CU) × 100 aspirin (C9H8O4) in the Sample solution taken:

rU = peak response of aspirin from the Sample Result = CU × (F/100)solution

CU = nominal concentration of aspirin in the SamplerS = peak response of aspirin from the Standardsolution (mg/mL)solution

F = percentage of the labeled amount of aspirinCS = concentration of USP Aspirin RS in the(C9H8O4) in the portion of Boluses taken, asStandard solution (mg/mL)determined in the AssayCU = nominal concentration of aspirin in the Sample

Calculate the percentage of salicylic acid (C7H6O3) insolution (mg/mL)• (IRA 1-Jan-2017)the portion of Boluses taken:

Result = (rU/rS) × (CS/C) × 100

2016 The United States Pharmacopeial Convention All Rights Reserved.

C171442-M6245-CHM32015, Rev. 0 20161118

Interim Revision Announcement2 Aspirin Official January 1, 2017

rU = peak response of salicylic acid from the Sample • USP REFERENCE STANDARDS ⟨11⟩solution USP Aspirin RS

rS = peak response of salicylic acid from the USP Salicylic Acid RS•

.Salicylic acid standard solution• (IRA 1-Jan-2017)

CS = concentration of USP Salicylic Acid RS in the•

.Salicylic acid standard solution• (IRA 1-Jan-2017)

(mg/mL)C = actual concentration of aspirin in the Sample

solutionAcceptance criteria: NMT 0.3%

ADDITIONAL REQUIREMENTS• PACKAGING AND STORAGE: Preserve in tight containers.• LABELING: Label Boluses to indicate that they are for vet-

erinary use only.

2016 The United States Pharmacopeial Convention All Rights Reserved.

C171442-M6245-CHM32015, Rev. 0 20161118