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Revision Bulletin

Official December 1, 2010Cefdinir1

Relative standard deviation: NMT 1.0%, Standard solution

Analysis

Cefdinir

Samples: Standard solution and Sample solution

Calculate the quantity (mg/mg) of cefdinir (C14H13N5O5S2) in the portion of Cefdinir taken:Result = (rU/rS) ´ (CS/CU) ´ P rU= peak response from the Sample solution rS= peak response from the Standard solution CS= concentration of the Standard solution (mg/mL) C14H13N5O5S2 395.41CU= concentration of the Sample solution (mg/mL)

5-Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, 7-[[(2-P= purity of USP Cefdinir RS (mg/mg)

amino-4-thiazolyl)(hydroxyimino)acetyl]amino]-3-ethenyl-8-Acceptance criteria:

940±1030 mg/mg on the anhydrous

oxo-, [6R-[6a, 7b(Z)]]-;basis

IMPURITIES

vinyl-5-thia-1-azabicyclo [4.2.0] oct-2-ene-2-carboxylic acid,

·RESIDUE ON IGNITION á281ñ: NMT 0.20%

7 2 -(Z)-oxime [91832-40-5].

·HEAVY METALS, Method II á231ñ: 10 ppm

DEFINITION·ORGANIC IMPURITIES

Cefdinir contains NLT 940 mg/mg and NMT 1030 mg/mg ofProcedure

cefdinir (C14H13N5O5S2), calculated on the anhydrous basis.Solution A, Solution B, Buffer solution, Solution C, and

Solution D: Prepare as directed in the Assay.

IDENTIFICATION

Solution E: To 1000 mL of Solution C add 0.4 mL of Solu-

·A. INFRARED ABSORPTION á197Mñ

tion D. ·B. The retention time of the major peak of the Sample solu- Solution F: Acetonitrile, methanol, Solution C, and Solution tion corresponds to that of the Standard solution, as obtained D (300:200:500:0.4) in the Assay. System suitability solution A: 15 mg/mL of cefdinir from the Sample solution, diluted with Solution C ASSAY System suitability solution B: 1.5 mg /mL of cefdinir from

·PROCEDURE

System suitability solution A, diluted with Solution C Solution A: 14.2 mg/mL of anhydrous dibasic sodium System suitability solution C: Transfer about 30 mg of phosphate USP Cefdinir RS and 2 mg of USP Cefdinir Related Com- Solution B: 13.6 mg/mL of monobasic potassium phosphate pound A RS to a 20-mL volumetric flask, dissolve in 3 mL Buffer solution: Combine appropriate amounts of Solution A of Buffer solution, and dilute with Solution C to volume. and Solution B (about 2:1) to obtain a solution with a pH of Sample stock solution: 10 mg/mL of Cefdinir in Buffer 7.0. solution Solution C: Dilute tetramethylammonium hydroxide (10%) Sample solution: 1.5 mg/mL of cefdinir from the Sample with water to obtain a 0.1% solution. Adjust with 10% stock solution, in Solution C. [NOTEÐPrepare fresh immedi- phosphoric acid to a pH of 5.5. ately before use.]

Solution D: 37.2 mg/mL of edetate disodium

Mobile phase: See Table 1.

Mobile phase: Acetonitrile, methanol, Solution C, and Solu- tion D (300:200:4500:2)

Table 1

System suitability solution: 0.2 mg/mL of USP Cefdinir RS and 0.5 mg/mL of USP Cefdinir Related Compound A RS in

TimeSolution ESolution F

Buffer solution

(min)(%)(%) Standard solution: 0.2 mg/mL of USP Cefdinir RS in Buffer 0955
solution 2955

Sample solution:

0.2 mg/mL of Cefdinir in Buffer solution

227525

Chromatographic system

325050

(See Chromatography á621ñ, System Suitability.)

Mode: LC375050

Detector: UV 254 nm

38955

Column: 4.6-mm ´ 15-cm; 5-mm packing L1

58955

Column temperature: 40°

Flow rate: 1 mL/min

Chromatographic system

Injection size: 5 mL

(See Chromatography á621ñ, System Suitability.)

System suitability

Mode: LC

Samples: System suitability solution and Standard solution

Detector: UV 254 nm

[NOTEÐUSP Cefdinir Related Compound A RS should pro-

Column: 4.6-mm ´ 15-cm; 5-mm packing L1

duce four peaks.]

Column temperature: 40°

Tailing factor: NMT 1.5 for cefdinir, System suitability

Flow rate: 1 mL/min

solution

Injection size: 10 mL

Resolution: NLT 1.2 between the second peak of cefdinir

System suitability

related compound A and cefdinir, System suitability solution Samples: System suitability solution A, System suitability solution B, and System suitability solution C [NOTEÐUSP Cefdinir Related Compound A RS should pro- duce four peaks.] ã2010 The United States Pharmacopeial ConventionAll Rights Reserved.

Revision Bulletin

2CefdinirOfficial December 1, 2010

[NOTEÐThe relative retention time of the third peak fromTable 2 (Continued) cefdinir related compound A is NLT 1.1, relative to the

RelativeAcceptance

cefdinir peak, System suitability solution C.]

RetentionCriteria,

Suitability requirements

NameTimeNMT (%)

Response ratio: The response of cefdinir in System suit-

Impurity H

h (2 peaks)1.61, 1.640.5 (sum of 2) ability solution B is between 7% and 13% of that from

Any other individual,

System suitability solution A.

unidentified impurityÐ0.2 Column efficiency: NLT 7000 theoretical plates for Total impuritiesÐ3.0cefdinir, System suitability solution C Tailing factor: NMT 3.0 for cefdinir, System suitabilitya solution Cb Relative standard deviation: NMT 2.0% for cefdinir, no)acetamide.

System suitability solution Cc

Analysis

yl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid.

Sample: Sample solutiond

[NOTEÐRecord the chromatogram for NLT 40 min.] Calculate the percentage of each impurity in the portion of yl]acetic acid.

Cefdinir taken:e

Result = (rU/rT) ´ 100

yl}acetamide. f rU= peak response of each impurity from the Sample cyclo[4.2.0]oct-2-ene-2-carboxylic acid. solution g rT= sum of all the peak responses from the Sample oxo-3-vinyl-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. solution h

Acceptance criteria: See Table 2.

Table 2

SPECIFIC TESTS

RelativeAcceptance

·OPTICAL ROTATION, Specific Rotation á781Sñ: -61° to -67° at

RetentionCriteria,

20°

NameTimeNMT (%)

Sample solution: 10 mg/mL in Buffer Solution, as obtained

Impurity A

a

0.100.5in the Assay

Impurity B

b

0.120.5

Impurity C

c

0.740.7

Change to read:

Cefdinir related com-0.85, 0.93, 1.11,

pound A d (4 peaks)1.140.7 (sum of 4) ·WATER DETERMINATION, Method I á921ñ: NMT 2.0% for anhy-

Impurity E

e

1.220.5drous; 4.0%±

8.5% for hydrated forms

[NOTEÐFor this monograph, the term ªhydrated formsº re-

Impurity F

f

1.360.5

fers to several known forms of Cefdinir.] (RB 1-Dec-2010)

Impurity G

g

1.510.7

[NOTEÐUse a mixture of formamide and methanol (2:1) as a the solvent.] b no)acetamide.

ADDITIONAL REQUIREMENTS

c ·PACKAGING AND STORAGE: Preserve in tight, light-resistant yl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. containers. d

·USP REFERENCE STANDARDS á11ñ

USP Cefdinir RS

yl]acetic acid.

USP Cefdinir Related Compound A RS

e yl}acetamide. trahydro-1H-furo[3,4-d][1,3]thiazin-2-yl]acetic acid (other f three stereo isomers are also present in this RS). cyclo[4.2.0]oct-2-ene-2-carboxylic acid.

C14H15N5O6S2413.43

g oxo-3-vinyl-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. h ã2010 The United States Pharmacopeial ConventionAll Rights Reserved.quotesdbs_dbs17.pdfusesText_23

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