Mesalamine Delayed-Release Tablets
If you find any inaccurate information, please let us know by providing your feedback here
Tóm tắt nội dung
This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition
Issued and maintained by the United States Pharmacopeial Convention (USP)
1 DEFINITION
Mesalamine Delayed-Release Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of mesalamine (C7H7NO3).
2 IDENTIFICATION
Change to read:
A. SPECTROSCOPIC IDENTIFICATION TESTS 〈197〉 , Infrared Spectroscopy: 197A or (USP 1-Dec-2024) 197K
Sample: To about 50 mL of water add a quantity of finely powdered Tablets, nominally equivalent to about 800 mg of mesalamine. Boil the mixture for about 5 min, with constant stirring. Filter the hot solution, and allow the filtrate to cool. Collect the precipitated crystals, and dry at about 110°.
Acceptance criteria: Meet the requirements
B. The retention time of the mesalamine peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
3 ASSAY
Change to read:
3.1 PROCEDURE
Buffer: Dissolve 1.8 g of monobasic potassium phosphate and 4.7 g of sodium 1-octanesulfonate in 1 L of water. Adjust with phosphoric acid to a pH of 2.1.
Mobile phase: Methanol and Buffer (25:75)
Standard solution: 0.2 mg/mL of USP Mesalamine RS in 0.01 N hydrochloric acid
Sample stock solution: Nominally 0.8 mg/mL of mesalamine from Tablets prepared as follows. Finely powder Tablets (NLT 10). Transfer a portion nominally equivalent to about 400 mg of mesalamine to a 500-mL volumetric flask. Add 50 mL of 0.5 N hydrochloric acid, and sonicate for 15 min. Add 350 mL of water and stir vigorously for NLT 60 min. Dilute with water to volume, and mix.
Sample solution: Nominally 0.2 mg/mL of mesalamine in water, from Sample stock solution. Pass a portion of the solution through a suitable filter of 0.45-µm or finer pore size.
3.1.1 Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 220 nm
Column: 4.6-mm × 25-cm; 5-µm packing L7
Column temperature: 30°
Flow rate: 1.5 mL/min
Injection volume: 10 µL
Run time: NLT 1.3 times the retention time of mesalamine
3.1.2 System suitability
Sample: Standard solution
Suitability requirements
Tailing factor: NMT 2.0
Relative standard deviation: NMT 1.0%
3.1.3 Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response of mesalamine from the Sample solution
rS = peak response of mesalamine from the Standard solution
CS = concentration of USP Mesalamine RS in the Standard solution (mg/mL)
CU = nominal concentration of mesalamine in the Sample solution (mg/mL)
(USP 1-Dec-2024)
Acceptance criteria: 90.0%–110.0%
4 PERFORMANCE TESTS
4.1 DISSOLUTION 〈711〉
4.1.1 Test 1
Solution A: Transfer about 43.35 g of monobasic potassium phosphate and 1.65 g of sodium hy droxide to a 2-L volumetric flask. Dissolve in and dilute with water to volume, and mix. Adjust with 1 N sodium hydroxide or phosphoric acid to a pH of 6.0, and mix.
Solution B: Transfer 133.6 g of sodium hy droxide to a 2-L volumetric flask, dissolve in and dilute with water to volume, and mix.
Medium
Acid stage: 500 mL of 0.1 N hydrochloric acid
Buffer stages: 900 mL of Solution A
Apparatus 2
Acid stage: 100 rpm Buffer stage 1: 100 rpm
Buffer stage 2: 50 rpm Times
Acid stage: 2 h Buffer stage 1: 1 h
Buffer stage 2: 90 min
Acid stage: After 2 h of operation, withdraw an aliquot of the fluid, discard the remaining solution, and retain the Tablets in proper order so that each will be returned later to its respective vessel. Blot the Tablets with a paper towel to dry, and proceed immediately as directed in Buffer stage 1.
Standard solution: A known concentration of USP Mesalamine RS in Medium, equivalent to about 1% of the labeled amount of mesalamine (C7H7NO3)
Sample solution: Filter portions of the solution under test, and suitably dilute with Medium, if necessary.
Instrumental conditions
Mode: UV
Analytical wavelength: 302 nm (maximum absorbance)
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (AU/AS) × CS × V × (1/L) × 100
AU = absorbance of the Sample solution
AS = absorbance of the Standard solution
CS = concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 500 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: See Table 1. Continue testing through all levels unless the results conform at an earlier level.
Buffer stage 1
[NOTE—Use Solution A that has been equilibrated to a temperature of 37 ± 0.5°.]
Transfer Solution A to each of the dissolution vessels, and place each Tablet from the Acid stage into its respective vessel. After 1 h, remove a 50-mL aliquot, and proceed immediately as directed in Buffer stage 2.
Standard solution: A known concentration of USP Mesalamine RS in Medium, equivalent to about 1% of the labeled amount of mesalamine (C H NO )
Sample solution: Filter portions of the solution under test, and suitably dilute with Medium, if necessary. Instrumental conditions
Mode: UV
Analytical wavelength: 330 nm (maximum absorbance) Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (AU/AS) × CS × V × (1/L) × 100
AU = absorbance of the Sample solution
AS = absorbance of the Standard solution
CS = concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 900 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: See Table 1. Continue testing through all levels unless the results conform at an earlier level.
Table 1
Buffer stage 2: Add 50 mL of Solution B to each dissolution vessel to adjust to a pH of 7.2, and continue the run. Standard solution: A known concentration of USP Mesalamine RS in Medium
Sample solution: Filter portions of the solution under test, and suitably dilute with Medium, if necessary.
Instrumental conditions
Mode: UV
Analytical wavelength: 332 nm (maximum absorbance)
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (AU/AS) × CS × V × (1/L) × 100
AU = absorbance of the Sample solution
AS = absorbance of the Standard solution
CS = concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 900 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: NLT 80% (Q ) of the labeled amount of mesalamine (C7H7NO3) is dissolved. The requirements are met if the quantities dissolved from the product conform to Dissolution 〈711〉 , Acceptance Table 4. Continue testing through all levels unless the results conform at an earlier level.
4.1.2 Test 2
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.
Solution A: pH 6.4 phosphate buffer (21.7 g/L of monobasic potassium phosphate and 0.8 g/L of sodium hydroxide in water, adjusted with 5 N sodium hy droxide or phosphoric acid to a pH of 6.4)
Solution B: 3.3 N sodium hydroxide (136 g/L of sodium hydroxide in water)
Medium
Acid stage: 750 mL of 0.1 N hydrochloric acid
Buffer stage 1: 950 mL of Solution A
Buffer stage 2: 960 mL of pH 7.2 phosphate buffer Apparatus 2: 100 rpm
Times
Acid stage: 2 h Buffer stage 1: 1 h
Buffer stage 2: 1, 2, and 6 h
Acid stage
After 2 h of operation, withdraw a portion of the solution under test, discard the remaining solution, and retain the Tablets in proper order so that each will be returned later to its respective vessel. Blot the Tablets with a paper towel to dry and proceed immediately as directed in Buffer stage 1.
Standard solution: 0.016 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve.
Sample solution: Pass a portion of the solution under test through a suitable filter of 0.45-μm pore size and discard the first few milliliters.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 302 nm
Blank: Medium Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (A /A ) × C × V × (1/L) × 100
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 750 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: NMT 1% of the labeled amount of mesalamine (C7H7NO3) is dissolved.
Buffer stage 1
[NOTE—Use Solution A that has been equilibrated to a temperature of 37 ± 0.5°.]
Transfer Solution A to each of the dissolution vessels, and place each Tablet from the Acid stage into its respective vessel. After 1 h, withdraw a 10-mL aliquot and proceed immediately as directed in Buffer stage 2.
Standard solution: 0.0125 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve.
Sample solution: Pass a portion of the withdrawn solution under test through a suitable filter of 0.45-μm pore size and discard the first few milliliters.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 330 nm Blank: Medium
Analysis: Proceed as directed in the Analysis at Acid stage, using the Medium for Buffer stage 1. Tolerances: NMT 1% of the labeled amount of mesalamine (C7H7NO3) is dissolved.
Buffer stage 2
To adjust the pH of 940 mL of Solution A to a pH of 7.2, transfer 20 mL of Solution B into each dissolution vessel from Buffer stage 1 and start the dissolution immediately.
At the end of the specified time point, withdraw 10 mL of the solution under test from each dissolution vessel and replace with 10 mL of Medium for Buffer stage 2.
Standard solution: 0.0315 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve.
Sample solution: Dilute 2.5 mL of the withdrawn solution under test with Medium to 100 mL. Pass through a suitable filter of 0.45-μm pore size and discard the first few milliliters.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 332 nm Blank: Medium
Analysis
Samples: Standard solution and Sample solution
Calculate the concentration (C ) of mesalamine (C7H7NO3) in the sample withdrawn from the vessel at each time point (i):
Result = (A /A ) × C × D
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
D = dilution factor for the Sample solution, 40
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved at each time point i:
Result = C × V × (1/L) × 100 Result = [(C × V) + (C × V )] × (1/L) × 100
Result = {(C × V) + [(C + C ) × V ]} × (1/L) × 100
= concentration of mesalamine in the portion of sample withdrawn at time point i (mg/mL)
V = volume of the Medium, 960 mL L = label claim (mg/Tablet)
= volume of the solution under test withdrawn at each time point (i) during Buffer stage 2, 10 mL
Tolerances: See Table 2.
Table 2
4.1.3 Test 3
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 3.
Solution A: pH 6.4 phosphate buffer [20.4 g/L of potassium phosphate, monobasic and 1.6 g/L of sodium hydroxide in water, adjusted with 1 N (or 5 N) sodium hy droxide or phosphoric acid to a pH of 6.4]
Solution B: pH 7.2 phosphate buffer [20.4 g/L of potassium phosphate, monobasic and 4.2 g/L of sodium hy droxide in water, adjusted with 1 N (or 5 N) sodium hydroxide or phosphoric acid to a pH of 7.2]
Medium
Acid stage: 0.1 N hydrochloric acid, 750 mL
Buffer stage 1: Solution A, 950 mL
Buffer stage 2: Solution B, 960 mL Apparatus 2
Acid stage: 100 rpm
Buffer stage 1: 100 rpm
Buffer stage 2: 100 rpm
Times
Acid stage: 2 h Buffer stage 1: 1 h
Buffer stage 2: 0.5 h and 1.5 h
Buffer: 5 g/L of potassium phosphate, monobasic in water, adjusted with phosphoric acid to a pH of 2.0 ± 0.05 Mobile phase: Acetonitrile and Buffer (20:80)
Diluent: Solution B and water (33:67)
Standard solution: 1.25 mg/mL of USP Mesalamine RS in Diluent. Sonicate to dissolve. Sample solutions
Acid stage: Place 1 Tablet in each vessel containing Medium, Acid stage. At the specified Times, withdraw a portion of the solution under test using a suitable filter of 10-μm pore size. Centrifuge if necessary. Remove the Tablets from solution, dry the Tablets with a paper towel, and retain in the proper order. Proceed as directed in Buffer stage 1.
Buffer stage 1: Transfer each Tablet from Acid stage into the respective vessel containing Medium, Buffer stage 1. At the specified Times, withdraw a portion of the solution under test using a suitable filter of 10-μm pore size. Centrifuge if necessary. Remove the Tablets from solution, dry the Tablets with a paper towel, and retain in the proper order. Proceed as directed in Buffer stage 2.
Buffer stage 2: Transfer each Tablet from Buffer stage 1 into the respective vessel containing Medium, Buffer stage 2. At the specified Times, withdraw a portion of the solution under test using a suitable filter of 10-μm pore size. Centrifuge if necessary.
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 330 nm
Column: 4.6-mm × 15-cm; 5-µm packing L9
Column temperature: 30°
Flow rate: 1.2 mL/min
Injection volume: 5 µL for Acid stage and Buffer stage 1; 2 μL for Buffer stage 2
Run time: NLT 2.5 times the retention time of mesalamine
System suitability
Sample: Standard solution Suitability requirements
Tailing factor: NMT 2.0
Relative standard deviation: NMT 2.0% Analysis
Acid stage
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (r /r ) × C × V × (1/L) × 100
= peak response of mesalamine from the Sample solution
= peak response of mesalamine from the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 750 mL
L = label claim (mg/Tablet)
Buffer stage 1: Proceed as directed for the Acid stage except the volume of Medium is 950 mL. Buffer stage 2
Samples: Standard solution and Sample solution
Calculate the concentration (C ) of mesalamine (C7H7NO3) in the sample withdrawn from the vessel at each time point (i) as shown in Table 4:
Result = (r /r ) × C
= peak response of mesalamine from the Sample solution
= peak response of mesalamine from the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved at each time point (i) as shown in Table 4: Result = (C × V) × (1/L) × 100
Result = {[C × (V − V )] + (C × V )} × (1/L) × 100
= concentration of mesalamine in the portion of sample withdrawn at each time point (i) (mg/mL)
V = volume of Medium, 960 mL L = label claim (mg/Tablet)
= volume of the Sample solution withdrawn at each time point (i) (mL)
Tolerances
Acid stage: See Table 3. Buffer stage 1: See Table 3.
Table 3
Buffer stage 2: See Table 4.
Table 4
Test 4: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 4. Solution A: 0.2 M phosphate buffer (76.0 g/L of sodium phosphate, tribasic, dodecahydrate in water) Medium
Acid stage: 0.1 N hydrochloric acid, 750 mL
Buffer stage 1: pH 6.4 phosphate buffer (after Acid stage, adjust with the addition of 200 mL of Solution A to the Medium, Acid stage to a pH of 6.4), 950 mL
Buffer stage 2: pH 7.2 phosphate buffer (after Buffer stage 1, adjust with the addition of about 10 mL of 2 M sodium hydroxide solution to the Medium, Buffer stage 1 to a pH of 7.2), 960 mL
Apparatus 2: 100 rpm Times
Acid stage: 2 h Buffer stage 1: 1 h
Buffer stage 2: 1, 2, and 6 h
Acid stage
Standard solution: 0.016 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve, if necessary.
Sample solution: At the specified Times, withdraw about 10 mL of the solution under test, pass through a suitable filter of 0.45-μm pore size, and collect the filtrate by discarding the first few milliliters. Replace with about 10 mL of Medium.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 302 nm Cell: 1 cm
Blank: Medium
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (A /A ) × C × V × (1/L) × 100
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 750 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: NMT 1% of the labeled amount of mesalamine (C7H7NO3) is dissolved. Buffer stage 1
Standard solution: 0.012 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve, if necessary.
Sample solution: At the specified Times, withdraw about 10 mL of the solution under test, pass through a suitable filter of 0.45-μm pore size, and collect the filtrate by discarding the first few milliliters. Replace with about 10 mL of Medium.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 331 nm Cell: 1 cm
Blank: Medium
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (A /A ) × C × V × (1/L) × 100
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 950 mL
L = label claim of mesalamine (mg/Tablet)
Tolerances: NMT 1% of the labeled amount of mesalamine (C7H7NO3) is dissolved. Buffer stage 2
Standard solution: 0.025 mg/mL of USP Mesalamine RS in Medium. Sonicate to dissolve, if necessary.
Sample solution: At the specified Times, withdraw about 10 mL of the solution under test, pass through a suitable filter of 0.45-μm pore size, and collect the filtrate by discarding the first few milliliters. Dilute 2.0 mL of the filtrate with Medium to 100 mL. Replace with about 10 mL of Medium.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 331 nm Cell: 1 cm
Blank: Medium Analysis
Samples: Standard solution and Sample solution
Calculate the concentration (C ) of mesalamine (C7H7NO3) in the sample withdrawn from the vessel at each time point (i):
Result = (A /A ) × C × D
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
D = dilution factor for the Sample solution, 50
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved at each time point (i):
Result = C × V × (1/L) × 100 Result = [(C × V) + (C × V )] × (1/L) × 100
Result = {(C × V) + [(C + C ) × V ]} × (1/L) × 100
= concentration of mesalamine in the portion of sample withdrawn at each time point (i) (mg/mL)
V = volume of Medium, 960 mL L = label claim (mg/Tablet)
= volume of the solution under test withdrawn at each time point (i) during Buffer stage 2, 10 mL
Tolerances: See Table 5.
Table 5
Test 5: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 5. Medium
Acid stage: 0.1 N hy drochloric acid; 750 mL, deaerated
Buffer stage 1: pH 6.4 phosphate buffer (prepare a solution of 6.8 g/L of potassium phosphate, monobasic and 0.55 g/L of sodium hy droxide in water, and adjust with either 2.5 N sodium hy droxide solution or phosphoric acid to a pH of 6.4); 950 mL, deaerated
Buffer stage 2: pH 7.2 phosphate buffer (after withdrawing 40 mL of solution from Buffer stage 1 at the specified Times, add 50 mL of 0.4 N sodium hydroxide solution to the remaining solution, and adjust with either 4 N sodium hydroxide or phosphoric acid to a pH of 7.2); 960 mL
Apparatus 2: 100 rpm Times
Acid stage: 2 h Buffer stage 1: 1 h
Buffer stage 2: 1, 2, and 6 h
Diluent: pH 7.2 phosphate buffer prepared as follows. Prepare a solution of 6.8 g/L of potassium phosphate, monobasic and 1.3 g/L of sodium hy droxide in water, and adjust with either 0.4 N sodium hy droxide solution or phosphoric acid to a pH of 7.2.
Standard stock solution: 0.4 mg/mL of USP Mesalamine RS in Diluent. Sonicate to dissolve, if necessary. Acid stage
Standard solution: 0.016 mg/mL of USP Mesalamine RS in Medium, Acid stage from Standard stock solution
Sample solution: Place 1 Tablet in each vessel containing Medium, Acid stage. At the specified Time, withdraw 10 mL of the solution under test. Pass through a suitable filter of 0.45-μm pore size and discard the first 5 mL of the filtrate. Drain the remaining Medium, Acid stage and retain the Tablet in the respective vessel.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 302 nm
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (A /A ) × C × V × (1/L) × 100
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 750 mL
L = label claim (mg/Tablet)
Tolerances: See Table 6 .
Buffer stage 1
Standard solution: 0.012 mg/mL of USP Mesalamine RS in Medium, Buffer stage 1 from Standard stock solution
Sample solution: After draining the Medium, Acid stage, transfer Medium, Buffer stage 1 to each dissolution vessel already containing the Tablet from the Acid stage. At the specified Time, withdraw 40 mL of the solution and proceed immediately as directed in Buffer stage 2. Pass through a suitable filter of 0.45-μm pore size and discard the first 5 mL of the filtrate.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 330 nm Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of mesalamine (C7H7NO3) dissolved:
Result = (A /A ) × C × V × (1/L) × 100 + Q
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
V = volume of Medium, 950 mL
L = label claim (mg/Tablet)
= percentage of the labeled amount of mesalamine dissolved in Acid stage
Tolerances: See Table 6 .
Table 6
Buffer stage 2
Standard solution: 0.04 mg/mL of USP Mesalamine RS in Diluent from Standard stock solution
Sample stock solution: Continue the test from Buffer stage 1. Add 50 mL of 0.4 N sodium hydroxide solution to each dissolution vessel. Adjust with either 4 N sodium hy droxide or phosphoric acid to a pH of 7.2 and start the dissolution for Buffer stage 2. At the specified Times, withdraw about 10 mL (for manual sampling) or 7 mL (for autosampler) of the solution under test and replace with 10 mL (for manual sampling) or 7 mL (for autosampler) of Medium for Buffer stage 2. Pass through a suitable filter of 0.45-μm pore size and discard the first 5 mL of the filtrate. The nominal concentration of the solution is about 1.25 mg/mL of mesalamine.
Sample solution: Nominally 0.0375 mg/mL of mesalamine in Diluent from Sample stock solution. Pass through a suitable filter of 0.45-μm pore size and discard the first 5 mL of the filtrate.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〈857〉.) Mode: UV
Analytical wavelength: 330 nm Analysis
Samples: Standard solution and Sample solution
Calculate the concentration (C ) of mesalamine (C H NO ) in the sample withdrawn from the vessel at each time point (i):
Result = (A /A ) × C × D
= absorbance of the Sample solution
= absorbance of the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
D = dilution factor for the Sample solution, 33.3
Calculate the percentage of the labeled amount of mesalamine (C H NO ) dissolved at each time point (i):
Result = C × V × (1/L) × 100 + Q + Q Result = [(C × V) + (C × V )] × (1/L) × 100 + Q + Q
Result = {(C × V) + [(C + C ) × V ]} × (1/L) × 100 + Q + Q
= concentration of mesalamine in the portion of sample withdrawn at each time point (mg/mL)
V = volume of Medium, 960 mL L = label claim (mg/Tablet)
= percentage of the labeled amount of mesalamine dissolved in Acid stage
= percentage of the labeled amount of mesalamine dissolved in Buffer stage 1
= volume of the Sample solution withdrawn at each time point, 10 mL (for manual sampling) or 7 mL (for autosampler)
Tolerances: See Table 7.
Table 7
The percentages of the labeled amount of mesalamine (C H NO ) dissolved at the times specified conform to Dissolution
〈711〉 , Acceptance Table 2.
UNIFORMITY OF DOSAGE UNITS 〈905〉 , Weight Variation: Meet the requirements
5 IMPURITIES
Change to read:
ORGANIC IMPURITIES
Buffer, Mobile phase, Sample stock solution, and Sample solution: Prepare as directed in the Assay. Standard solution: 0.002 mg/mL of USP Mesalamine RS in 0.01 N hydrochloric acid
Sensitivity solution: 0.1 µg/mL of USP Mesalamine RS in 0.01 N hy drochloric acid, prepared from Standard solution Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 220 nm
Column: 4.6-mm × 25-cm; 5-µm packing L7 Column temperature: 30°
Flow rate: 1.5 mL/min
Injection volume: 30 µL
Run time: NLT 2.8 times the retention time of mesalamine System suitability
Samples: Standard solution and Sensitivity solution Suitability requirements
Relative standard deviation: NMT 5.0%, Standard solution
Signal-to-noise ratio: NLT 10, Sensitivity solution Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of any unspecified degradation product in the portion of Tablets taken:
Result = (r /r ) × (C /C ) × 100
= peak response of any unspecified degradation product from the Sample solution
= peak response of mesalamine from the Standard solution
= concentration of USP Mesalamine RS in the Standard solution (mg/mL)
= nominal concentration of mesalamine in the Sample solution (mg/mL)
Acceptance criteria: The reporting threshold is 0.05%. Any unspecified degradation product: NMT 0.10% Total degradation products: NMT 2.0% (USP 1-Dec-2024)
6 ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in tight containers. Store at controlled room temperature.
LABELING: When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used. Change to read:
USP REFERENCE STANDARDS 〈11〉
USP Mesalamine RS
(USP 1-Dec-2024)
