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hao8431

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[交流] 埃索美拉唑钠 药典标准

埃索美拉唑钠 有没有药典标准呀
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没有的话，自己生产的话这标准是参考 埃索美拉唑镁 还是 奥美拉唑钠
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1楼 2011-08-30 14:30:40
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匿名

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31楼2016-01-15 16:59:41
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zpc910905

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hao8431(金币+1):谢谢参与
我还以为是奥美拉唑……
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2楼2011-08-30 14:35:50
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ronalbeck

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以下是USP34版友原料药镁盐的标准
Esomeprazole Magnesium
(es'' oh mep' ra zole mag nee' zee um).
C34H36MgN6O6S2·3H2O Trihydrate: 767.17
C34H36MgN6O6S2 Anhydrous: 713.12
1H-Benzimidazole,5-methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridinyl)methyl]sulfinyl],
magnesium salt (2:1), trihydrate;
5-Methoxy-2-[(S)-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfinyl]benzimidazole,
magnesium salt (2:1), trihydrate [217087-09-7].
DEFINITION
Esomeprazole Magnesium contains NLT 98.0% and NMT 102.0% of C34H36MgN6O6S2,
calculated on the anhydrous basis.
IDENTIFICATION
• A. INFRARED ABSORPTION 197K
• B. The Sample solution, prepared and tested as directed in the test for Content of
Magnesium, exhibits a significant absorption at 285.2 nm.
ASSAY
• PROCEDURE
Solution A: Dissolve 0.725 g of monobasic sodium phosphate and 4.472 g of anhydrous
dibasic sodium phosphate in 300 mL of water, and dilute with water to 1000 mL. Dilute
250 mL of this solution with water to 1000 mL. If necessary, adjust with phosphoric acid
to a pH of 7.6.
Solution B: Mix 11 mL of 0.25 M tribasic sodium phosphate with 22 mL of 0.5 M dibasic
sodium phosphate, and dilute with water to 100 mL.
Mobile phase: Acetonitrile and Solution A (7:13)
Standard solution: Transfer 10 mg of USP Omeprazole RS to a 200-mL volumetric flask,
and dissolve in about 10 mL of methanol. Add 10 mL of Solution B, and dilute with water
to volume. [NOTE—This solution contains 0.05 mg/mL of omeprazole. ]
Sample solution: Transfer 10 mg of Esomeprazole Magnesium to a 200-mL volumetric
flask, and dissolve in about 10 mL of methanol. Add 10 mL of Solution B, and dilute with
water to volume. [NOTE—This solution contains 0.05 mg/mL of esomeprazole
magnesium. ]
Chromatographic system
(See Chromatography 621 , System Suitability.)
Mode: LC
Detector: UV 280 nm
Column: 4.0-mm × 12.5-cm or a 4.6-mm × 15-cm; 5-μm packing L7. [NOTE—
Alternatively, a 3.9-mm × 15-cm column that contains 4-μm packing L1 may be used. ]
Flow rate: 1 mL/min
Injection size: 20 μL
System suitability
Sample: Standard solution
Suitability requirements
Column efficiency: NLT 2000 theoretical plates
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of C34H36MgN6O6S2 in the portion of Esomeprazole
Magnesium taken:
Result = (rU/rS) × (CS/CU) × [Mr1/(2 × Mr2)] × 100
Acceptance criteria: 98.0%–102.0% on the anhydrous basis
OTHER COMPONENTS
• CONTENT OF MAGNESIUM
Lanthanum solution: Transfer 58.7 g of lanthanum oxide into a 1000-mL volumetric flask,
wet the substance with some water, and dissolve by cautious addition of 250 mL of
hydrochloric acid in 20- to 30-mL portions, cooling between the additions. Add water
while stirring, cool to room temperature, and dilute with water to volume. [NOTE—Store
the solution in a plastic bottle. ]
Standard stock solution: 1000 μg/mL of magnesium in water, from a commercially
prepared atomic absorption standard solution. [NOTE—Store the solution in a plastic
bottle. ]
Standard solution A: Transfer 10.0 mL of Standard stock solution to a 500-mL volumetric
flask, add 50 mL of 1 N hydrochloric acid, and dilute with water to volume. Transfer 20.0
rU = = peak response from the Sample solution
rS = = peak response from the Standard solution
CS = = concentration of omeprazole in the Standard
solution (mg/mL)
CU = = concentration of Esomeprazole Magnesium
in the Sample solution (mg/mL)
Mr1 = = molecular weight of esomeprazole
magnesium, 713.12
Mr2 = = molecular weight of omeprazole, 345.42
mL of this solution to a 200-mL volumetric flask, and dilute with water to volume. [NOTE—
This solution contains 2 μg/mL of magnesium. ]
Standard solution B: Combine 5.0 mL of Standard solution A and 4.0 mL of Lanthanum
solution, and dilute with water to 100.0 mL (0.1 μg/mL).
Standard solution C: Combine 10.0 mL of Standard solution A and 4.0 mL of Lanthanum
solution, and dilute with water to 100.0 mL (0.2 μg/mL).
Standard solution D: Combine 15.0 mL of Standard solution A and 4.0 mL of Lanthanum
solution, and dilute with water to 100.0 mL (0.3 μg/mL).
Standard solution E: Combine 20.0 mL of Standard solution A and 4.0 mL of Lanthanum
solution, and dilute with water to 100.0 mL (0.4 μg/mL).
Standard solution F: Combine 25.0 mL of Standard solution A and 4.0 mL of Lanthanum
solution, and dilute with water to 100.0 mL (0.5 μg/mL). [NOTE—Concentrations of the
Standard solutions and the Sample solution may be modified to fit the linear or working
range of the instrument. When using instruments with a linear calibration graph, the
number of Standard solutions can be reduced. ]
Blank solution: Transfer 4.0 mL of Lanthanum solution to a 100-mL volumetric flask, and
dilute with water to volume.
Sample solution: Transfer 250 mg of Esomeprazole Magnesium to a 100-mL volumetric
flask, add 20 mL of 1 N hydrochloric acid, swirl until dissolved, and dilute with water to
volume. Allow to stand for 30 min. Transfer 10.0 mL of this solution to a 200-mL
volumetric flask, and dilute with water to volume. Transfer 10.0 mL of the solution to
another 100-mL volumetric flask, add 4.0 mL of Lanthanum solution, and dilute with water
to volume.
Spectrometric conditions
(See Spectrophotometry and Light-Scattering 851 .)
Mode: Atomic absorption spectrophotometer
Flame: Air–acetylene
Analytical wavelength: 285.2 nm
Analysis
Samples: Standard solution B, Standard solution C, Standard solution D, Standard
solution E, Standard solution F, Blank solution, and Sample solution
Determine the concentration, Cs, in μg/mL, of magnesium in the Sample solution using
the calibration graph.
Calculate the percentage of magnesium in the portion of Esomeprazole Magnesium
taken:
Result = (CS/CU) × (100/(100 F)) × 100
CS = = content of magnesium in the Sample
solution as calculated above (μg/mL)
CU = = concentration of Esomeprazole Magnesium
in the Sample solution (μg/mL)
F = = content of water in Esomeprazole
Acceptance criteria: 3.30%–3.55%, on anhydrous basis
IMPURITIES
Organic Impurities
• PROCEDURE 1
Solution A: 0.725 g of monobasic sodium phosphate and 4.472 g of anhydrous dibasic
sodium phosphate in 300 mL of water, and dilute with water to 1000 mL. Dilute 250 mL of
this solution with water to 1000 mL. If necessary, adjust with phosphoric acid to a pH of
7.6.
Mobile phase: Acetonitrile and Solution A (11:29). [NOTE—To improve the resolution, the
composition may be changed to 1:3, if necessary. ]
System suitability solution: 1 mg of USP Omeprazole RS and 1 mg of USP Omeprazole
Related Compound A RS in 25 mL of Mobile phase. [NOTE—Omeprazole Related
Compound A is omeprazole sulfone. ]
Sample solution: 4 mg of Esomeprazole Magnesium in 25 mL of Mobile phase. [NOTE—
Prepare this solution fresh. ]
Chromatographic system
(See Chromatography 621 , System Suitability.)
Mode: LC
Detector: UV 280 nm
Column: 4.0-mm × 12.5-cm or a 4.6-mm × 15-cm; 5-μm packing L7. [NOTE—
Alternatively, a 3.9-mm × 15-cm column that contains 4-μm packing L1 may be used. ]
Flow rate: 0.8–1 mL/min
Injection size: 50 μL
System suitability
Sample: System suitability solution
[NOTE—For relative retention times, see Impurity Table 1. ]
Suitability requirements
Resolution: NLT 3 between omeprazole related compound A and omeprazole
Analysis
Sample: Sample solution
Record the chromatogram for at least 4.5 times the retention time of the omeprazole
peak, and measure the peak responses. Identify the impurities based on the retention
times shown in Impurity Table 1.
Calculate the percentage of any individual impurity in the portion of Esomeprazole
Magnesium taken:
Result = (rU/rT) × 100
Magnesium, as determined in Specific Tests,
Water Determination (%)
rU = = peak response for each impurity
= = sum of all peak responses
Acceptance criteria
Individual impurities: See Impurity Table 1.
Total impurities: NMT 0.5%
Impurity Table 1
• PROCEDURE 2: ENANTIOMERIC PURITY
Solution A: Mix 70 mL of 1 M monobasic sodium phosphate with 20 mL of 0.5 M dibasic
sodium phosphate, and dilute with water to 1000 mL. Dilute 250 mL of this solution with
water to 1000 mL.
Diluent: Mix 11 mL of 0.25 M tribasic sodium phosphate with 22 mL of 0.5 M dibasic
sodium phosphate, and dilute with water to 1000 mL.
Mobile phase: Acetonitrile and Solution A (3:17)
System suitability solution: 2 mg of USP Omeprazole RS in 10 mL of Diluent. Dilute 1.0
mL of this solution with Diluent to 50 mL.
Sample solution: 40 mg of Esomeprazole Magnesium in 5 mL of methanol, and dilute
with Diluent to 25 mL. Dilute 1 mL of this solution with Diluent to 50 mL.
Chromatographic system
(See Chromatography 621 , System Suitability.)
Mode: LC
Detector: UV 302 nm
Column: 4.0-mm × 10-cm; packing L41
Flow rate: 0.6 mL/min
Injection size: 20 μL
System suitability
Sample: System suitability solution
Suitability requirements
Resolution: NLT 3 between the enantiomer peaks. [NOTE—The elution order is the Renantiomer,
followed by the esomeprazole peak, which is the S-enantiomer. ]
Analysis
rT
Name
Relative
Retention
Time
Acceptance
Criteria,
NMT (%)
Omeprazole N-oxide a 0.45 0.1
Omeprazole sulfoneb (related compound A) 0.8 0.2
Any other individual impurities — 0.1
Omeprazole 1.0 —
a 4-Methoxy-2-[[(RS)-(5-methoxy-1H-benzimidazol-2-yl)sulfinyl]methyl]-3,5-
dimethylpyridine 1-oxide.
b 5-Methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-1Hbenzimidazole.
Sample: Sample solution
Calculate the percentage of the R-enantiomer in the portion of Esomeprazole
Magnesium taken:
Result = (rU/rS) × 100
Acceptance criteria: NMT 0.2% of the R-enantiomer
SPECIFIC TESTS
• WATER DETERMINATION, Method I 921 : 6.0%–8.0%
• COLOR OF SOLUTION
Sample solution: 20 mg/mL of Esomeprazole Magnesium in methanol
Analysis: Determine the absorbance of this solution at 440 nm, in 1-cm cells, using
methanol as the blank.
Acceptance criteria: NMT 0.2
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers, protected from light. Store at room
temperature.
• USP REFERENCE STANDARDS 11
USP Esomeprazole Magnesium RS
USP OMEPRAZOLE RS
USP OMEPRAZOLE RELATED COMPOUND A RS
Omeprazole sulfone, 5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-
1H-benzimidazole.
C17H19N3O4S 361.42 [CAS-88546-55-8].
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
USP34–NF29 Page 2741
Pharmacopeial Forum: Volume No. 35(3) Page 550
Chromatographic Column—
ESOMEPRAZOLE MAGNESIUM
rU = = peak response for the R-enantiomer
rS = = sum of the peak responses for
esomeprazole and R-enantiomer
Topic/Question Contact Expert Committee
Monograph Elena Gonikberg, Ph.D.
Principal Scientific
Liaison
1-301-816-8251
(SM32010) Monographs - Small Molecules
3
Reference
Standards
RS Technical Services
1-301-816-8129
rstech@usp.org
Chromatographic columns text is not derived from, and not part of, USP 34 or NF 29
还有EP7.0里面是三水合物的标准，如果需要可以联系我，或留下邮箱我把标准发给你！
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3楼2011-08-30 14:44:06
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chfpl_1

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最好参考埃索美拉唑镁，有USP，bp，ep的标准
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4楼2011-08-30 14:50:28
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