USP Medicines Compendium - Eflornithine Topical Cream - 2013-01-16

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Eflornithine Topical Cream

Final Authorized Version 1.0

DEFINITION

Eflornithine Topical Cream contains NLT 95.0% and NMT 105.0% of the labeled amount of eflornithine hydrochloride (C6H12F2N2O2 HCl).

Performance-Based Monograph

(Contains tests, procedures, and acceptance criteria for the material under test. It also includes the criteria-based procedures that

define the equivalence criteria necessary to demonstrate that anAcceptable Procedureis equivalent to the Reference Procedures.)

IDENTIFICATION

A.The response of eflornithine hydrochloride from the Sample solutioncorresponds to that of the Standard solution, as obtained in

theAssay.

ASSAY

PROCEDURE

Standard solution: MC Eflornithine Hydrochloride CRM in an appropriate diluent

Sample solution: Dilute an aliquot of Topical Cream in an appropriate diluent to obtain a concentration approximately the same as

that of the Standard solution.

Analytical system: Use a procedure validated as described in the MCgeneral chapterAssessingValidation Parameters for

Reference and Acceptable Procedures.

System performance requirements

Precision:Meets the requirements for 97.0%103.0%

Accuracy:Meets the requirements for 97.0%103.0%

Specificity:Meets the requirements

Range:Meets the requirementsAnalysis

Samples:Standard solution and Sample solution

Calculate the percentage of the labeled amount of eflornithine hydrochloride in the Sample solution. [NOTEIf the procedurethat is used separately quantifies the eflornithine enantiomers, the calculation of content should be based on their sum.]

Result = (rU/rS) (CS/CU) 100

rU = peak response from the Sample solution

rS = peak response from the Standard solution

CS = concentration of MC Eflornithine Hydrochloride CRM in the Standard solution

CU

= nominal concentration of eflornithine hydrochloride in the Sample solution

Acceptance criteria: 95.0%105.0%

IMPURITIES

ELEMENTAL IMPURITIES :Meets the requirements

RESIDUAL SOLVENTS : Meets the requirements

ORGANICIMPURITIES

Standard solution: MC Eflornithine Hydrochloride CRM and all appropriate MC Impurity RMs, at concentrations corresponding to the

Acceptance criteriaof the impurity, in an appropriate diluent

Sample solution: Dilute or extract an aliquot of Topical Cream in an appropriate diluent to obtain a concentration approximately the

same as that of the Standard solution.

Analytical system: Use a procedure validated as described in MCgeneral chapterAssessingValidation Parameters for Reference

and Acceptable Procedures.

System performance requirements

Precision:Meets the requirements

Accuracy:Meets the requirements
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Specificity:Meets the requirements

Analysis

Samples:Standard solution and Sample solution

Calculate the percentage of each impurity in the Sample solution. [NOTEIf the procedure that is used separately quantifies theeflornithine enantiomers, the calculation of impurity content should be compared to their sum.]


rU = peak response of each impurity from the Sample solution

rS = peak response of each Impurity RM from the Standard solution.[NOTEIf no Impurity RMs are available, usethe peak response of eflornithine.]

CS = concentration of the standard material in the Standard solution

CU = nominal concentration of eflornithine hydrochloride in the Sample solution

Acceptance criteria

Any individual impurity: NMT 0.15%

Total impurities:NMT 2.0%

PERFORMANCE TESTS

MINIMUM FILL : Meets the requirements

ADDITIONAL REQUIREMENTS

REFERENCE STANDARDS

MC Eflornithine Hydrochloride CRM

REFERENCE PROCEDURES

(This section provides detailed descriptions of procedures that may be used for the evaluation of the material under test. These

procedures have been fully validated and the data is available on the MC website.)

ASSAY

PROCEDURE

Solution A:10 mM ammonium acetate in water. Adjust with acetic acid to a pH of 5.3.

Mobile phase: Acetonitrile and Solution A (4:1)

Diluent:Mobile phase

Standard solution: 5.0 mg/mL of MC Eflornithine Hydrochloride CRM in Diluent

Sample solution:Weigh an appropriate quantity of Topical Cream, extract with Diluent, and sonicate for 35 minutes. Dilute with

Diluent, and pass through a 0.45-m filter to obtain a final eflornithine hydrochloride concentration of about 5.0 mg/mL.

Chromatographic system

(See Chromatography , System Suitability.)

Mode:LC

Detector:PDA (scan 200400 nm). [NOTECalculations should be based on the chromatograms collected at 210 nm.]

[NOTETo confirm the absence of co-eluting known and unknown impurity peaks, substitute the detector used below in the testfor Organic Impurities.]

Column: 4.6-mm 25-cm; 5-m packing L1 (similar to Thermo Hypersil Hilic)

Flow rate:1 mL/min

Injection volume:20 L

System suitability

Sample:Standard solution

Suitability requirements

Relative standard deviation:NMT 1.0% for the eflornithine hydrochloride peak

Analysis

Samples:Standard solutionand Sample solution

Calculate the percentage of eflornithine hydrochloride in the portion of Topical Cream taken:


rU = peak response of eflornithine hydrochloride from the Sample solution


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rS = peak response of eflornithine hydrochloride from the Standard solution

CS = concentration of MC Eflornithine Hydrochloride CRM in the Standard solution. [NOTEThe potency of theReference Material is included in this term.]

CU = concentration of eflornithine hydrochloride in the Sample solution

IMPURITIES

ORGANICIMPURITIES

Solution A,Mobile phase,Diluent, Sample solutionand Chromatographic system:Proceed as directed in ReferenceProcedures, Assay.

Detector:PDA and MS in series.

MS source:ES scan (+ and )

MS conditions

Capillary:3.00 kv

Cone:15.0 v

Extractor:2.0 v

Rf lense:0.1 v

Source temperature:80

Desolvation temperature:450

Standard solution: 5.0 mg/mL of MC Eflornithine Hydrochloride CRM and all appropriate MC Impurity RMs, at concentrations

corresponding to theAcceptance criteriaof the impurity in Diluent

System suitability

Sample:Standard solution

Suitability requirements

Relative standard deviation:NMT 1.0% for the eflornithine hydrochloride peak

Analysis

Samples:Standard solutionand Sample solution

Calculate the percentage of each impurity in the portion of Topical Cream taken: [NOTEWhere an impurity other than thoseincluded in the Standard solutionis found in the Sample solution, the peak response and concentration of eflornithine in the

Standard solutionis used for the calculation.]


rU = peak response of each impurity from the Sample solution

rS = peak response of each impurity from the Standard solution.

CS = concentration of each impurity in the Standard solution. [NOTEThe potency of the Reference Material isincluded in this term.]

CU = concentration of eflornithine hydrochloride in the Sample solution

Source URL (modified on 2013/01/16 - 1:45pm): https://mc.usp.org/monographs/eflornithine-topical-cream-1-0

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USP Medicines Compendium - Eflornithine Topical Cream - 2013-01-16