Famotidine Tablets
DEFINITION
Famotidine Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of famotidine (C8H15N7O2S3).
IDENTIFICATION
• A. Thin-Layer Chromatographic Identification Test 〈201〉
Standard solution: 4 mg/mL of USP Famotidine RS in glacial acetic acid
Sample solution: Transfer a portion of finely powdered Tablets, equivalent to about 40 mg of
famotidine, to a 10-mL volumetric flask. Dissolve in glacial acetic acid with the aid of sonication, dilute with glacial acetic acid to volume, and centrifuge to get a clear liquid.
Adsorbent: 0.25-mm layer of chromatographic silica gel mixture
Application volume: 10 µL
Developing solvent system: Ethyl acetate, methanol, toluene, and ammonium hydroxide
(40:25:20:2)
Analysis: Allow the spots to dry, and develop the plate in a paper-lined chromatographic chamber equilibrated with Developing solvent system for about 1 h before u. Allow the chromatogram to develop until the solvent front has moved about 15 cm. Remove the plate, air-dry, and examine the plate under short-wavelength UV light.
Acceptance criteria: The principal spot from the Sample solution corresponds in appearance and RF value to that of the Standard solution.
• B. The retention time of the major peak in the Sample solution corresponds to that in the
Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Buffer: Dissolve 13.6 g of sodium acetate trihydrate in 750 mL of water. Add 1 mL of
triethylamine, adjust with glacial acetic acid to a pH of 6.0, and dilute with water to 1 L.
Mobile pha: Acetonitrile and Buffer (7:93)
Diluent: Dissolve 6.8 g of monobasic potassium phosphate in 750 mL of water, adjust with 1 M potassium hydroxide to a pH of 6.0, and dilute with water to 1 L.
System suitability stock solution: Transfer 10 mg of famotidine to a 50-mL volumetric flask. Add
1 mL of 0.1 N hydrochloric acid, heat at 80° for 30 min, and cool to room temperature. Add
2 mL
of 0.1 N sodium hydroxide, heat at 80° for 30 min, cool to room temperature, and neutralize by adding 1 mL of 0.1 N hydrochloric acid. Dilute with Diluent to volume. Transfer 10 mL of this solution to a parate 50-mL volumetric flask containing 5 mg of famotidine dissolved in 8 mL of methanol. Dilute with Diluent to volume. Transfer 25 mL of this solution to a 50-mL volumetric
flask, and dilute with Diluent to volume. [Note—This solution is stable for up to 1 month.] System suitability solution: Transfer 1–1.5 mL of the System suitability stock solution to a suitable container, add 1 drop of hydrogen peroxide solution, and mix well.
[Note—Prepare fresh daily.]
Standard solution: Transfer 10 mg of USP Famotidine RS to a 100-mL volumetric flask, add 20 mL of methanol, and sonicate for 5 min. Dilute with Diluent to volume.
海葵是什么
Sample solution: Transfer NLT 10 Tablets to a 1-L volumetric flask. Add 200 mL of Diluent, and swirl to erode the Tablets. Add 200 mL of methanol, and stir by mechanical means at 300 rpm for 1 h. Dilute with Diluent to volume, mix, and filter. Quantitatively dilute a portion of the clear filtrate with Diluent to obtain a solution containing about 0.1 mg/mL of famotidine. Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 275 nm
Column: 4.6-mm × 15-cm; packing L1
Column temperature: 40°
Flow rate: 1.4 mL/min
Injection size: 50 µL
System suitability
Samples: System suitability solution and Standard solution
普世牧首Suitability requirements
[Note—Identify peaks using Table 1.]
Resolution: NLT 1.3 between the famotidine sulfamoyl propanamide and famotidine peaks, and NLT 1.3 between the famotidine and famotidine propanamide peaks, System suitability solution
Capacity factor: NLT 2.0 for the famotidine peak, System suitability solution
Relative standard deviation: Less than 2.0%, Standard solution
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of famotidine (C8H15N7O2S3) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
rU=peak respon from the Sample solution
东方之珠合唱rS=peak respon from the Standard solution
CS=concentration of USP Famotidine RS in the Standard solution (mg/mL)
CU=nominal concentration of famotidine in the Sample solution (mg/mL)
Acceptance criteria: 90.0%–110.0%
PERFORMANCE TESTS
Change to read:
• Dissolution 〈711〉
Medium: pH 4.5, 0.1 M phosphate buffer (13.6 g/L of monobasic potassium phosphate); 900 mL Apparatus 2: 50 rpm
Time: 30 min
传单制作
dufuDetermine the amount of C8H15N7O2S3 dissolved using one of the following methods.
Spectrophotometric method
Standard solution: USP Famotidine RS in Medium in a concentration similar to the one
expected in the Sample solution
Sample solution: Pass a portion of the sample under test through a suitable filter.
喜居宝地Instrumental conditions
(See Ultraviolet-Visible Spectroscopy 〉(CN 1-May-2016).)
Mode: UV
Analytical wavelength: 265 nm
泉州医保中心Chromatographic method
Buffer, Mobile pha, and Chromatographic system: Proceed as directed in the Assay.
Standard solution: 0.14 mg/mL of USP Famotidine RS in Medium. Dilute this solution with
Medium to obtain a solution containing (L/900) mg/mL, where L is the Famotidine Tablet label claim, in mg.
Sample solution: Pass a portion of the solution under test through a suitable filter.
System suitability
Sample: Standard solution
Suitability requirements
Capacity factor: Greater than 2.0
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the amount of famotidine (C8H15N7O2S3) dissolved:
Result = (rU/rS) × (CS/L) × V × 100
rU=peak respon from the Sample solution
rS=peak respon from the Standard solution
CS=concentration of USP Famotidine RS in the Standard solution (mg/mL)
L=label claim, mg/Tablet
V=volume of Medium, 900 mL
Tolerances: NLT 75% (Q) of the labeled amount of famotidine (C8H15N7O2S3) is dissolved.
For Tablets labeled as chewable
Proceed as directed for either of the methods specified above, except for the following:
Time: 45 min
Tolerances: NLT 80% (Q) of the labeled amount of famotidine (C8H15N7O2S3) is dissolved.
For Tablets labeled as film-coated
Proceed as directed for either of the methods specified above, except for the following:
Time: 30 min
Tolerances: NLT 80% (Q) of the labeled amount of famotidine (C8H15N7O2S3) is dissolved.
企业代码查询
• Uniformity of Dosage Units 〈905〉: Meet the requirements
IMPURITIES
• Organic Impurities
Mobile pha, Diluent, System suitability solution, Standard solution, Sample solution,
Chromatographic system, and System suitability: Proceed as directed in the Assay.
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
rU=peak area of each impurity from the Sample solution
rS=peak area of famotidine from the Standard solution
CS=concentration of USP Famotidine RS in the Standard solution (mg/mL)
CU=nominal concentration of famotidine in the Sample solution (mg/mL)
F=relative respon factor for each impurity (e Table 1)
Acceptance criteria: See Table 1.
Table 1
Name Relative
Retention
Time
Relative
Respon
Factor
Acceptance
Criteria
NMT (%)
Famotidine sulfoxide a0.4 1.0 1.0
Famotidine propionic acid
(famotidine related compound F)b0.7 1.00.5
Famotidine sulfamoyl propanamide
(famotidine related compound C)c0.8 1.00.5
Famotidine 1.0——
Famotidine propanamide
(famotidine related compound D)d 1.2 1.30.5
Total impurities—— 1.5
a 3-[[2-(Diaminomethyleneamino)thiazol-4-yl]methylsulfinyl]-N′-
sulfamoylpropanimidamide.
b 3-[[2-(Diaminomethyleneamino)thiazol-4-yl]methylthio]propanoi
c acid.
c 3-[[2-(Diaminomethyleneamino)thiazol-4-yl]methylthio]-N-sulfamoylpropanamide.
d 3-[[2-(Diaminomethyleneamino)thiazol-4-yl]methylthio]propanamide.
ADDITIONAL REQUIREMENTS
• Packaging and Storage: Prerve in well-clod, light-resistant containers. Store at controlled room temperature.
• USP Reference Standards 〈11〉
