埃索美拉唑钠盐(原料药)标准 USP MC - Esomeprazole Sodium - 2012-07-23
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Omeprazole N-oxide, 4-methoxy-2-[[(RS)-(5-methoxy-1H-benzimidazol-2-yl)sulphinyl]methyl]-3,5-dimethylpyridine 1-oxide. USP Omeprazole Impurity F RS
1,3-Dimethyl-8-methoxy-12-thioxopyrido[1’,2’:3,4] imidazo[1,2-a] benzimidazol-2(12H)-one. USP Omeprazole Impurity G RS
ASSAY • Procedure
Solution A: 10 mM ammonium acetate in water. Adjust with ammonium hydroxide solution to a pH of 7.0. Solution B: Methanol and acetonitrile (1:1) Mobile phase: See Table 1.
Esomeprazole sodium is a white to almost white, crystalline powder. It is soluble in water and methylene chloride; freely soluble in ethanol.
Performance-Based Monograph (Contains tests, procedures, and acceptance criteria for the material under test. It also includes the criteria-based procedures necessary to demonstrate that an Acceptable Procedure is equivalent to the Reference Procedures.)
Omeprazole sulfone, 5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-1H-benzimidazole. USP Omeprazole Impurity B RS
5-Methoxy-2-1H-benzimidazol-2-thiol. USP Omeprazole Impurity E RS
1,3-Dimethyl-9-methoxy-12-thioxopyrido[1’,2’:3,4] imidazo[1,2-a] benzimidazol-2(12H)-one. USP Omeprazole Impurity I RS
Omeprazole sulfone N-oxide, 4-methoxy-2-[[(5-methoxy-1H-benzimidazol-2-yl)sulphonyl]methyl]-3,5-dimethylpyridine 1-oxide. USP R-Omeprazole RS
(See Chromatography <621>, System Suitability.) Mode: LC
Result = (rU/rS) × (CS/CU) × 100
rU = response of each impurity from the Sample solution rS = response of each USP Impurity RS from the Standard solution. [Note—If no USP Impurity RSs are available, use the response of esomeprazole.] CS = concentration of standard material in the Standard solution CU = concentration of Esomeprazole Sodium in the Sample solution Acceptance criteria R-Omeprazole: NMT 0.10% Any individual impurity: NMT 0.10% Total impurities: NMT 2.0%
Precision: Meets the requirements Accuracy: Meets the requirements Specificity: Meets the requirements Range: Meets the requirements Analysis
Samples: Standard solution and Sample solution Calculate the percentage of esomeprazole sodium (C17H19N3NaO3S) in the Sample solution:
ASSAY • Procedure
Standard solution: USP Esomeprazole Sodium CRM in an appropriate diluent Sample solution: Esomeprazole Sodium in an appropriate diluent Analytical system: Use a procedure validated as described in MC general chapter Assessing Validation Parameters for Reference and Acceptable Procedures <10>. System performance requirements
DEFINITION Esomeprazole Sodium contains NLT 98.0% and NMT 102.0% of esomeprazole sodium (C17H19N3NaO3S), calculated on the dried basis.
IDENTIFICATION • A. Infrared Absorption <197K> • B. Identification Tests—General, Sodium <191>
IMPURITIES • Residue on Ignition <281>: NMT 0.1% • Elemental Impurities <232>: Proceed as directed in the chapter. • Residual Solvents <467>: Proceed as directed in the chapter. • Organic Impurities
Time (min) 0 30 35 45 47 50
Table 1
Solution A (%) 60 45 30 30 60 60
SoΒιβλιοθήκη Baiduution B (%) 40 55 70 70 40 40
System suitability solution: 0.01 mg/mL each of USP Esomeprazole Sodium CRM and USP Omeprazole Impurity A RS in methanol Standard solution: 0.2 mg/mL of USP Esomeprazole Sodium CRM in methanol Sample solution: 0.2 mg/mL of Esomeprazole Sodium in methanol Chromatographic system
SPECIFIC TESTS • Water Determination, Method I <921>
Acceptance criteria: 6.0%–8.0%
ADDITIONAL REQUIREMENTS • Reference Standards <11>
USP Esomeprazole CRM USP Omeprazole Impurity A RS
Standard solution: USP Esomeprazole Sodium CRM and all appropriate USP Impurity RSs, at concentrations corresponding to the
Acceptance criteria of the impurity, in an appropriate diluent Sample solution: Esomeprazole Sodium in an appropriate diluent Analytical system: Use a procedure validated as described in MC general chapter Assessing Validation Parameters for Reference and Acceptable Procedures <10>.
Result = (rU/rS) × (CS/CU) × 100
rU = response from the Sample solution rS = response from the Standard solution CS = concentration of the Standard solution CU = concentration of the Sample solution Acceptance criteria: 98.0%–102.0% on the anhydrous basis
Published on USP Medicines Compendium (https://www.usp-mc.org)
Esomeprazole Sodium For Comment Version 0.2
C17H19N3NaO3S
368.41
1H-Benzimidazole, 5-methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridinyl)methyl]sulfinyl]-, sodium salt; 5-Methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfinyl]-1H-benzimidazole, sodium salt [161796-78-7].
System performance requirements Precision: Meets the requirements Accuracy: Meets the requirements Ruggedness: Meets the requirements Specificity: Meets the requirements Analysis Samples: Standard solution and Sample solution Calculate the percentage of each impurity in the Sample solution:
5-Methoxy-2-[(R)-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfinyl]-1H-benzimidazole.
REFERENCE PROCEDURES (This section provides detailed descriptions of procedures that may be used for the evaluation of the material under test. These procedures have been fully validated, and the data is available on the MC website.)
1,3-Dimethyl-8-methoxy-12-thioxopyrido[1’,2’:3,4] imidazo[1,2-a] benzimidazol-2(12H)-one. USP Omeprazole Impurity G RS
ASSAY • Procedure
Solution A: 10 mM ammonium acetate in water. Adjust with ammonium hydroxide solution to a pH of 7.0. Solution B: Methanol and acetonitrile (1:1) Mobile phase: See Table 1.
Esomeprazole sodium is a white to almost white, crystalline powder. It is soluble in water and methylene chloride; freely soluble in ethanol.
Performance-Based Monograph (Contains tests, procedures, and acceptance criteria for the material under test. It also includes the criteria-based procedures necessary to demonstrate that an Acceptable Procedure is equivalent to the Reference Procedures.)
Omeprazole sulfone, 5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-1H-benzimidazole. USP Omeprazole Impurity B RS
5-Methoxy-2-1H-benzimidazol-2-thiol. USP Omeprazole Impurity E RS
1,3-Dimethyl-9-methoxy-12-thioxopyrido[1’,2’:3,4] imidazo[1,2-a] benzimidazol-2(12H)-one. USP Omeprazole Impurity I RS
Omeprazole sulfone N-oxide, 4-methoxy-2-[[(5-methoxy-1H-benzimidazol-2-yl)sulphonyl]methyl]-3,5-dimethylpyridine 1-oxide. USP R-Omeprazole RS
(See Chromatography <621>, System Suitability.) Mode: LC
Result = (rU/rS) × (CS/CU) × 100
rU = response of each impurity from the Sample solution rS = response of each USP Impurity RS from the Standard solution. [Note—If no USP Impurity RSs are available, use the response of esomeprazole.] CS = concentration of standard material in the Standard solution CU = concentration of Esomeprazole Sodium in the Sample solution Acceptance criteria R-Omeprazole: NMT 0.10% Any individual impurity: NMT 0.10% Total impurities: NMT 2.0%
Precision: Meets the requirements Accuracy: Meets the requirements Specificity: Meets the requirements Range: Meets the requirements Analysis
Samples: Standard solution and Sample solution Calculate the percentage of esomeprazole sodium (C17H19N3NaO3S) in the Sample solution:
ASSAY • Procedure
Standard solution: USP Esomeprazole Sodium CRM in an appropriate diluent Sample solution: Esomeprazole Sodium in an appropriate diluent Analytical system: Use a procedure validated as described in MC general chapter Assessing Validation Parameters for Reference and Acceptable Procedures <10>. System performance requirements
DEFINITION Esomeprazole Sodium contains NLT 98.0% and NMT 102.0% of esomeprazole sodium (C17H19N3NaO3S), calculated on the dried basis.
IDENTIFICATION • A. Infrared Absorption <197K> • B. Identification Tests—General, Sodium <191>
IMPURITIES • Residue on Ignition <281>: NMT 0.1% • Elemental Impurities <232>: Proceed as directed in the chapter. • Residual Solvents <467>: Proceed as directed in the chapter. • Organic Impurities
Time (min) 0 30 35 45 47 50
Table 1
Solution A (%) 60 45 30 30 60 60
SoΒιβλιοθήκη Baiduution B (%) 40 55 70 70 40 40
System suitability solution: 0.01 mg/mL each of USP Esomeprazole Sodium CRM and USP Omeprazole Impurity A RS in methanol Standard solution: 0.2 mg/mL of USP Esomeprazole Sodium CRM in methanol Sample solution: 0.2 mg/mL of Esomeprazole Sodium in methanol Chromatographic system
SPECIFIC TESTS • Water Determination, Method I <921>
Acceptance criteria: 6.0%–8.0%
ADDITIONAL REQUIREMENTS • Reference Standards <11>
USP Esomeprazole CRM USP Omeprazole Impurity A RS
Standard solution: USP Esomeprazole Sodium CRM and all appropriate USP Impurity RSs, at concentrations corresponding to the
Acceptance criteria of the impurity, in an appropriate diluent Sample solution: Esomeprazole Sodium in an appropriate diluent Analytical system: Use a procedure validated as described in MC general chapter Assessing Validation Parameters for Reference and Acceptable Procedures <10>.
Result = (rU/rS) × (CS/CU) × 100
rU = response from the Sample solution rS = response from the Standard solution CS = concentration of the Standard solution CU = concentration of the Sample solution Acceptance criteria: 98.0%–102.0% on the anhydrous basis
Published on USP Medicines Compendium (https://www.usp-mc.org)
Esomeprazole Sodium For Comment Version 0.2
C17H19N3NaO3S
368.41
1H-Benzimidazole, 5-methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridinyl)methyl]sulfinyl]-, sodium salt; 5-Methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfinyl]-1H-benzimidazole, sodium salt [161796-78-7].
System performance requirements Precision: Meets the requirements Accuracy: Meets the requirements Ruggedness: Meets the requirements Specificity: Meets the requirements Analysis Samples: Standard solution and Sample solution Calculate the percentage of each impurity in the Sample solution:
5-Methoxy-2-[(R)-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfinyl]-1H-benzimidazole.
REFERENCE PROCEDURES (This section provides detailed descriptions of procedures that may be used for the evaluation of the material under test. These procedures have been fully validated, and the data is available on the MC website.)