Cefdinir for Oral Suspension
DEFINITION
Cefdinir for Oral Suspension contains NLT 90.0% and NMT 110.0% of the labeled amount of cefdinir (C14H13N5O5S2). It may contain one or more suitable buffers, flavors, preservatives, stabilizing agents, sweeteners, and suspending agents.
IDENTIFICATION
Delete the following:
• A. Thin-Layer Chromatographic Identification Test 201
Buffer:
Prepare as directed in the Assay.
Standard solution:
600 µg/mL of USP Cefdinir RS in methanol and Buffer (3:1)
Sample solution:
Transfer an equivalent to 125 mg of cefdinir, from reconstituted Oral Suspension, to a 100-mL volumetric flask, add 50 mL of Buffer, and dilute with methanol to volume. Pass a portion through a suitable filter of 0.45-µm pore size, transfer 5.0 mL of the filtrate to a 10-mL volumetric flask, and dilute with methanol to volume.
Adsorbent:
0.25-mm layer of chromatographic silica gel, preconditioned with n-hexane and tetradecane (95:5)
Application volume:
10 µL
Developing solvent system:
Methanol and water (4:1)
Visualization:
Short-wavelength UV
Analysis
Samples:
Standard solution and Sample solution
Develop the chromatogram until the solvent front has moved about 15 cm. Remove the plate, and allow the solvent to evaporate.
Acceptance criteria:
The RF value of the principal spot from the Sample solution corresponds to that from the Standard solution.USP35
Change to read:
• A.USP35
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Buffer:
10.7 mg/mL of anhydrous dibasic sodium phosphate and 3.4 mg/mL of monobasic potassium phosphate in water. Adjust with phosphoric acid or sodium hydroxide to a pH of 7.0 ± 0.05 before final dilution.
Solution A:
7 mg/mL of citric acid monohydrate. Adjust with phosphoric acid to a pH of 2.0 ± 0.05.
Mobile phase:
Methanol, tetrahydrofuran, and Solution A (111:28:1000)
System suitability solution:
50 µg/mL of USP Cefdinir RS and 175 µg/mL of m-hydroxybenzoic acid in Buffer
Standard solution:
50 µg/mL of USP Cefdinir RS in Buffer
Sample solution:
Equivalent to 50 µg/mL of cefdinir, from constituted Cefdinir for Oral Suspension, in Buffer
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
3.9-mm × 15-cm; 4-µm packing L1
Flow rate:
1.4 mL/min
Injection size:
15 µL
System suitability
Samples:
Standard solution and System suitability solution
Suitability requirements
Resolution:
NLT 3.0 between cefdinir and m-hydroxybenzoic acid, System suitability solution
Tailing factor:
NMT 2.0 for cefdinir, System suitability solution
Relative standard deviation:
NMT 1.0% for cefdinir, Standard solution
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of cefdinir (C14H13N5O5S2) in the portion of Cefdinir for Oral Suspension taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
90.0%110.0%
PERFORMANCE TESTS
• Dissolution 711
Medium:
0.05 M phosphate buffer pH 6.8; 900 mL
Apparatus 2:
50 rpm
Time:
30 min
Detector:
UV 290 nm
Standard solution:
0.14 mg/mL of USP Cefdinir RS in Medium
Sample solution:
Transfer 5 mL, by weight, of the reconstituted Cefdinir for Oral Suspension into the vessel. After the appropriate time, withdraw a portion of the solution under test, and pass through a suitable filter of 0.45-µm pore size. Dilute a portion of each filtered sample with Medium as necessary to obtain a solution having a concentration of about 0.14 mg/mL of cefdinir.
Blank:
Medium
Analysis:
Determine the percentage of the labeled amount of cefdinir (C14H13N5O5S2) dissolved:
Result = (AU/AS) × [(CS × d × D × V)/W × L] × 100
Tolerances:
NLT 80% (Q) of the labeled amount of C14H13N5O5S2 is dissolved.
• Uniformity of Dosage Units 905 (for solids packaged in single-unit containers):
Meets the requirements
• Deliverable Volume 698 (for solids packaged in single-unit containers):
Meets the requirements
IMPURITIES
Change to read:
Organic Impurities
• Procedure
Solution A:
14.2 mg/mL of anhydrous dibasic sodium phosphate
Solution B:
13.6 mg/mL of monobasic potassium phosphate
Buffer:
Combine appropriate amounts of Solution A and Solution B (about 2:1) to obtain a solution with a pH of 7.0 ± 0.1.
Solution C:
Dilute tetramethylammonium hydroxide (10% aqueous) with water to obtain a 0.1% solution. Adjust with dilute phosphoric acid (1 in 10) to a pH of 5.5 ± 0.1.
Solution D:
37.2 mg/mL of edetate disodium
Solution E:
To 1000 mL of Solution C add 0.4 mL of Solution D.
Solution F:
Acetonitrile, methanol, Solution C, and Solution D (150:100:250:0.2)
Mobile phase:
See Table 1.
Table 1
System suitability stock solution 1:
40 µg/mL of USP Cefdinir Related Compound A RS in Solution C
System suitability stock solution 2:
40 µg/mL of USP Cefdinir Related Compound B RS in Buffer
System suitability solution:
Transfer 37.5 mg of USP Cefdinir RS to a 25-mL volumetric flask. Add about 10 mL of Buffer. Add 5.0 mL each of System suitability stock solution 1 and System suitability stock solution 2, and dilute with Solution C to volume.
Standard stock solution:
750 µg/mL of USP Cefdinir RS in Buffer
Standard solution:
15 µg/mL of USP Cefdinir RS, from the Standard stock solution in Solution C
Sample solution:
Transfer a quantity equivalent to 150 mg of cefdinir from constituted Cefdinir for Oral Suspension to a 100-mL volumetric flask. Dissolve in 30 mL of Buffer, and dilute with Solution C to volume.
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Column temperature:
40
Autosampler temperature:
4
Flow rate:
1 mL/min
Injection size:
10 µL
System suitability
Samples:
System suitability solution and Standard solution
Suitability requirements
Resolution:
NLT 1.5 between cefdinir and the third peak for USP Cefdinir Related Compound A RS, System suitability solution
Tailing factor:
NMT 1.5 for cefdinir related compound B, System suitability solution
Relative standard deviation:
NMT 2.0% for the cefdinir peak response, Standard solution
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Cefdinir for Oral Suspension taken:
Result = (rU/rS) × (CS/CU) × 100/F
Acceptance criteria:
See Table 2.
USP35
Table 2
SPECIFIC TESTS
• pH 791:
3.54.5
Delete the following:
• Loss on Drying 731:
Dry about 1 g over phosphorous pentoxide in a vacuum not exceeding 5 mm of mercury at 70 for 44.5 h: it loses NMT 1.0% of its weight.USP35
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight, light-resistant containers, and store at controlled room temperature.
• Labeling:
The label specifies the directions for the constitution of the powder and states the equivalent amount of C14H13N5O5S2 in a given volume of Cefdinir for Oral Suspension after constitution.
• USP Reference Standards 11
USP Cefdinir RS
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2541
Pharmacopeial Forum: Volume No. 36(6) Page 1515
|