Balsalazide Disodium Capsules
DEFINITION
Balsalazide Disodium Capsules contain NLT 90.0% and NMT 110.0% of the labeled amount of balsalazide disodium (C17H13N3Na2O6·2H2O).
IDENTIFICATION
• A.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
• B. Ultraviolet Absorption
Using a 0.2-cm cell, record the UV spectrum of the Sample solution, obtained in the Assay, in the range of 200400 nm: it exhibits maxima at about 261 nm and 357 nm.
ASSAY
• Procedure
Buffer:
Add 5 mL of triethylamine to 1000 mL of water, and adjust with phosphoric acid to a pH of 6.00 ± 0.1.
Mobile phase:
Acetonitrile and Buffer (1:4)
Diluent:
Water
Standard solution:
60 µg/mL of USP Balsalazide Disodium RS in Diluent. [NoteUse sonication as necessary. ]
Sample stock solution:
Transfer an equivalent to 150 mg of balsalazide disodium, from the Capsules contents, to a 100-mL volumetric flask, add 70 mL of Diluent, sonicate for 5 min, and dilute with Diluent to volume.
Sample solution:
60 µg/mL of balsalazide disodium, from the Sample stock solution, in Diluent. Pass a portion of this solution through a suitable filter, discarding the first 3 mL.
Chromatographic system
Mode:
LC
Detector:
UV 360 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Column temperature:
30
Flow rate:
1 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Column efficiency:
NLT 10,000 theoretical plates
Tailing factor:
NMT 2.0
Relative standard deviation:
NMT 2.0%
Analysis
Sample:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of C17H13N3Na2O6·2H2O in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
90.0%110.0%
IMPURITIES
Organic Impurities
• Procedure
Buffer:
Dissolve 2.7 g of monobasic potassium phosphate in 1000 mL of water, and adjust with 10% potassium hydroxide solution to a pH of 6.00 ± 0.1.
Diluent:
Water
Solution A:
Buffer
Solution B:
Acetonitrile
Sample solution:
Transfer an amount of finely crushed powder equivalent to 100 mg of balsalazide disodium to a 100-mL volumetric flask, add 70 mL of Diluent, sonicate for 5 min, and dilute with Diluent to volume. Pass a portion of this solution through a PVDF filter of 0.45-µm pore size.
Standard solution:
1.0 µg/mL of USP Balsalazide Disodium RS in Diluent
System suitability solution:
1.0 µg/mL of USP Balsalazide Disodium RS, 1.5 µg/mL of USP Balsalazide Related Compound A RS, 0.5 µg/mL of USP Balsalazide Related Compound B RS, and 0.5 µg/mL of USP Salicylic Acid RS in Diluent
Mobile phase:
See the gradient table below.
Chromatographic system
Mode:
LC
Detector:
UV 238 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Column temperature:
45
Flow rate:
1 mL/min
Injection size:
30 µL
System suitability
Samples:
Standard solution and System suitability solution
Suitability requirements
Resolution:
NLT 5 between balsalazide and balsalazide related compound B, System suitability solution
Relative standard deviation:
NMT 5.0%, Standard solution
Tailing factor:
NMT 1.5, Standard solution
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × (1/F)× 100
Acceptance criteria
Individual impurities:
See Impurity Table 1.
Reporting level for impurities:
0.05%
Total impurities:
NMT 1.0%. [NoteWhen reporting results for Individual impurities and Total impurities, disregard peaks corresponding to salicylic acid and balsalazide related compound B, as these impurities are controlled in the drug substance only. ]
Impurity Table 1
PERFORMANCE TESTS
• Dissolution 711
Medium:
pH 6.8 phosphate buffer; 900 mL
Apparatus 2:
50 rpm, with stainless steel wire helix sinkers
Time:
30 min
Detector:
UV 357 nm, with background correction at 590 nm
Path length:
0.02-cm flow cell
Blank:
Medium
Standard solution:
0.83 mg/mL of USP Balsalazide Disodium RS in Medium
Sample solution:
Pass a portion of the solution under test through a suitable filter of 20-µm pore size.
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C17H13N3Na2O6·2H2O dissolved:
Result = (AU/AS) × CS × V × (100/L)
Tolerances:
NLT 70% (Q) of the labeled amount of C17H13N3Na2O6·2H2O is dissolved.
• Uniformity of Dosage Units 905:
Meet the requirements
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight containers, and store at controlled room temperature.
• USP Reference Standards 11
USP Balsalazide Related Compound A RS
(E)-5-[(p-Carboxyphenyl)azo]-2-salicylic acid, disodium salt. C14H8N2O5Na2 330.12
USP Balsalazide Related Compound B RS
(E)-5-({m-[(2-Carboxyethyl)carbamoyl]phenyl}azo)-2-salicylic acid. C17H15N3O6 357.17
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2304
Pharmacopeial Forum: Volume No. 35(4) Page 832
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