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uu325

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[交流] 【求助】求助几个药品的国外质量标准

求助几个药品的国外质量标准

pramipexole，moxifloxacin，imatinib，sitafloxacin，linezolid
求助以上药品的国外质量标准，如USP,EP,JP,UK.
谢谢！
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1楼 2011-03-14 16:39:45
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dingjinglvde

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uu325(金币+4): 谢啦 2011-04-25 12:36:20
Moxifloxacin Hydrochloride
(mox'' i flox' a sin hye'' droe klor' ide)
  
C21H24FN3O4·HCl
437.89
(4aS-cis)-1-Cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-7-(octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl)-4-oxo-3-quinolinecarboxylic acid, monohydrochloride;     
1-Cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-3-quinolinecarboxylic acid, monohydrochloride     [186826-86-8].
DEFINITION
Moxifloxacin Hydrochloride contains NLT 98.0% and NMT 102.0% of C21H24FN3O4·HCl, calculated on the anhydrous basis.
IDENTIFICATION
•  A. Infrared Absorption 197K
•  B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
•  C. Identification Tests—General, Chloride 191: Meets the requirements
Sample solution:  To a solution (1 in 160) add diluted nitric acid, and filter.
ASSAY
•  Procedure
Buffer:  Dissolve 0.5 g of tetrabutylammonium hydrogen sulfate and 1.0 g of monobasic potassium phosphate in water, add 2 mL of phosphoric acid, dilute with water to 1000 mL, mix, and pass through a 0.45-µm filter.
Mobile phase:  Methanol and Buffer (7:18)
Diluent:  Add 20 mg of anhydrous sodium sulfite to 1000 mL of Buffer solution, mix gently, and pass through a 0.45-µm filter.
System suitability solution:  0.1 and 0.001 mg/mL of USP Moxifloxacin Hydrochloride RS and USP Moxifloxacin Related Compound A RS, respectively, in Diluent
Standard solution:  0.1 mg/mL of USP Moxifloxacin Hydrochloride RS in Diluent
Sample solution:  0.1 mg/mL of moxifloxacin hydrochloride in Diluent
Chromatographic system  
(See Chromatography 621, System Suitability.)
Mode:  LC
Detector:  UV 293 nm
Column:  4.0-mm × 25-cm; 5-µm packing L11
Flow rate:  0.9 mL/min
Temperature:  45
Injection size:  25 µL
System suitability  
Samples:  System suitability solution and the Standard solution
[Note—The relative retention times are about 1.0 and 1.2, respectively. ]
Suitability requirements  
Resolution:  NLT 1.5 between moxifloxacin and moxifloxacin related compound A, System suitability solution
Column efficiency:  NLT 4000 theoretical plates, Standard solution
Tailing factor:  NMT 2.0, Standard solution
Relative standard deviation:  NMT 2.0%, Standard solution
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of C21H24FN3O4·HCl in the portion of moxifloxacin hydrochloride taken:
Result = (rU/rS) × (CS/CU) × 100
rU = = peak response from the Sample solution
rS = = peak response from the Standard solution
CS = = concentration of USP Moxifloxacin Hydrochloride RS in the Standard solution (mg/mL)
CU = = nominal concentration of moxifloxacin hydrochloride in the Sample solution (mg/mL)

Acceptance criteria:  98.0%–102.0% on the anydrous basis
IMPURITIES
Inorganic Impurities  
•  Residue on Ignition 281: NMT 0.1%
•  Chloride and Sulfate, Sulfate 221
Analysis:  0.6 g shows no more sulfate than corresponds to 0.25 mL of 0.020 N sulfuric acid.
Acceptance criteria:  NMT 0.04%
Organic Impurities  
•  Procedure: [Note—Protect solutions from light. ]
Mobile phase and Diluent:  Prepare as directed in the Assay.
Blank solution:  Use the Diluent.
System suitability solution:  Prepare as directed in the Assay.
Sensitivity solution:  0.05 µg/mL of USP Moxifloxacin Hydrochloride RS from the Standard solution in Diluent
[Note—Store the Sensitivity solution under refrigeration and protected from light. ]
Standard solution:  2 µg/mL of USP Moxifloxacin Hydrochloride RS in Diluent
Sample solution:  Prepare as directed in the Assay.
Chromatographic system:  Proceed as directed in the Assay.
System suitability  
Samples:  System suitability solution, Sensitivity solution, and Standard solution
Suitability requirements  
Resolution:  NLT 1.5 between moxifloxacin and moxifloxacin related compound A, System suitability solution
Column efficiency:  NLT 4000 theoretical plates, Standard solution
Tailing factor:  NMT 2.0, Standard solution
Relative standard deviation:  NMT 2.0%, Standard solution
Signal-to-noise ratio:  NLT 10, Sensitivity solution
Analysis  
Samples:  Blank solution, Standard solution, and Sample solution
Calculate the percentage of each impurity in the portion of moxifloxacin hydrochloride taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
rU = = peak response of each impurity from the Sample solution
rS = = peak response of moxifloxacin hydrochloride from the Standard solution
CS = = concentration of USP Moxifloxacin Hydrochloride RS in the Standard solution (mg/mL)
CU = = nominal concentration of moxifloxacin hydrochloride in the Sample solution (mg/mL)  
F = = relative response factor (see Impurity Table 1)  

Acceptance criteria  
Individual impurities:  See Impurity Table 1.
Total impurities:  NMT 1.0%
Impurity Table 1
Name Relative
Retention
Time  Relative
Response
Factor Acceptance
Criteria,
NMT %
Moxifloxacin related compound Aa 1.15 1.0 0.1
6,8-Dimethoxyb 1.32 0.71 0.1
8-Ethoxyc 1.48 1.0 0.1
6-Methoxy-8-fluorod  1.71 1.0 0.1
8-Hydroxye  1.83 0.29 0.1
Other individual
impurity — 1.0 0.1
Total impurities — — 0.5
a   1-Cyclopropyl-6,8-difluoro-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
b   1-Cyclopropyl-6,8-dimethoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
c   1-Cyclopropyl-8-ethoxy-6-fluoro-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
d   1-Cyclopropyl-8-fluoro-6-methoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
e   1-Cyclopropyl-6-fluoro-8-hydroxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.  

SPECIFIC TESTS
•  Optical rotation, Specific rotation 781S
Sample:  10 mg/mL in acetonitrile and water (1:1)
Acceptance criteria:  125 to 138 at 20
•  Microbial Enumeration Tests 61 and Tests for Specified Microorganisms 62:
Total aerobic microbial count:  NMT 1000 cfu/g
Total combined molds and yeasts count:  NMT 100 cfu/g
•  pH 791:
Sample solution:  0.2 in 100
Acceptance criteria:  3.9–4.6
•  Water Determination Method Ia 921: NMT 4.5%
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in tight, light-resistant containers. Store at room temperature.
•  USP Reference Standards 11
USP Moxifloxacin Hydrochloride RS
USP Moxifloxacin Related Compound A RS
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Behnam Davani, Ph.D., M.B.A.
Senior Scientist
1-301-816-8394 (MDAA05) Monograph Development-Antivirals and Antimicrobials
61 Radhakrishna S Tirumalai, Ph.D.
Senior Scientific Liaison
1-301-816-8339 (MSA05) Microbiology and Sterility Assurance
62 Radhakrishna S Tirumalai, Ph.D.
Senior Scientific Liaison
1-301-816-8339 (MSA05) Microbiology and Sterility Assurance
Reference Standards Lili Wang, Technical Services Scientist
1-301-816-8129
RSTech@usp.org  

USP33–NF28 Page 3929
Pharmacopeial Forum: Volume No. 34(5) Page 1170
Chromatographic Column—  
MOXIFLOXACIN HYDROCHLORIDE
Chromatographic columns text is not derived from, and not part of, USP 33 or NF 28.
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