求助，急需USP39或USP38版的加巴喷丁胶囊标准

天池雪莲

哪位好心的大侠能提供一份USP38/USP39的Gabapentin Capsules/Gabapentin/Gabapentin Tables的标准以及BP2016的Gabapentin Capsules/Gabapentin/Gabapentin Tables的标准？？


非常感谢！！！！！

hfsr

Gabapentin Capsules
DEFINITION
Gabapentin Capsules contain NLT 90.0% and NMT 110.0% of the labeled amount of gabapentin (C9H17NO2 ).
IDENTIFICATION
•  A. Infrared Absorption 197K
Sample:  Empty the contents of NLT 10 Capsules, and grind to a fine powder. Use a quantity of the powder, equivalent to 2 mg of gabapentin, and 200 mg of potassium bromide.
Acceptance criteria:  Meet the requirements
•  B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
•  Procedure
Diluent:  1.2 g/L of monobasic potassium phosphate in water. Adjust with 5 N potassium hydroxide to a pH of 6.9.
Mobile phase :  Dissolve 1.2 g of monobasic potassium phosphate in 940 mL water. Adjust with 5 N potassium hydroxide to a pH of 6.9. Add 60 mL of acetonitrile and stir.
Standard solution:  4.0 mg/mL of USP Gabapentin RS in Diluent
Sample solution:  Nominally 4.0 mg/mL of gabapentin, from the contents of NLT 20 Capsules, equivalent to 100 mg of gabapentin, in Diluent. Sonication for about 60 s may be necessary to dissolve the contents.
Chromatographic system  
(See Chromatography 621 , System Suitability.)
Mode:  LC
Detector:  UV 210 nm
Column:  4.6-mm × 25-cm; 5-µm packing L7
Flow rate:  1.2 mL/min
Injection volume:  50 µL
System suitability  
Sample:  Standard solution
Suitability requirements  
Column efficiency:  NLT 7000 theoretical plates
Tailing factor:  NMT 2.0
Relative standard deviation:  NMT 2.0%
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of the labeled amount of gabapentin (C9H17NO2 ) in the portion of Capsules taken:
Result = ( r U / r S ) × ( C S / C U ) × 100

r U  = = peak response from the Sample solution  
r S  = = peak response from the Standard solution  
C S  = = concentration of USP Gabapentin RS in the Standard solution (mg/mL)
C U  = = nominal concentration of gabapentin in the Sample solution (mg/mL)

Acceptance criteria:  90.0%–110.0%
PERFORMANCE TESTS
•   Dissolution 711
Medium:  0.06 N hydrochloric acid (prepared by adding 51 mL of hydrochloric acid to 10 L of water); 900 mL
Apparatus 2:  50 rpm
Time:  20 min
Sample solution:  Filter a portion of the solution under test using a suitable filter of 0.45-µm pore size.
Mobile phase:  Prepare as directed in the Assay.
Standard solution:  0.0011L mg/mL of USP Gabapentin RS in the Medium, where L is the label claim in mg/Capsule
Chromatographic system   
(See Chromatography 621 , System Suitability.)
Mode:  LC
Detector:  UV 210 nm
Column:  4.6-mm × 25-cm; 5-µm packing L7
Flow rate:  1.2 mL/min
Injection volume:  100 µL
System suitability  
Sample:  Standard solution
Suitability requirements  
Column efficiency:  NLT 7000 theoretical plates
Tailing factor:  NMT 2.0
Relative standard deviation:  NMT 2.0%
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of the labeled amount of gabapentin (C9H17NO2 ) dissolved:
Result = ( r U / r S ) × C S × V × (1/L) × 100

r U  = = peak response from the Sample solution  
r S  = = peak response from the Standard solution  
C S  = = concentration of the Standard solution (mg/mL)
V  = = volume of the Medium in the dissolution vessel, 900 mL
L  = = label claim (mg/Capsule)

Tolerances:  NLT 80% (Q) of the labeled amount of gabapentin (C9H17NO2 ) is dissolved.
•   Uniformity of Dosage Units 905 : Meet the requirements
IMPURITIES
•  Organic Impurities
Diluent:  Prepare as directed in the Assay.
Solution A:  Dissolve 1.2 g of monobasic potassium phosphate in 940 mL water. Adjust with 5 N potassium hydroxide to a pH of 6.9. Add 60 mL of acetonitrile and stir.
Solution B:  Dissolve 1.2 g of monobasic potassium phosphate in 700 mL water. Adjust with 5 N potassium hydroxide to a pH of 6.9. Add 300 mL of acetonitrile and stir.
Mobile phase:  See Table 1.
Table 1
Time
(min) Solution A
(%) Solution B
(%)
0.0  100  0
4.0  100  0
45.0  0  100
45.1  100  0
50.0  100  0

Standard solution:  0.04 mg/mL each of USP Gabapentin RS and USP Gabapentin Related Compound A RS in Diluent
Sample solution:  Nominally 20 mg/mL of gabapentin, from the contents of NLT 20 Capsules, equivalent to 500 mg of gabapentin, in Diluent. Sonication for about 30 s may be necessary.
Chromatographic system   
(See Chromatography 621 , System Suitability.)
Mode:  LC
Detector:  UV 210 nm
Column:  4.6-mm × 25-cm; 5-µm packing L7
Flow rate:  1.5 mL/min
Injection volume:  50 µL
System suitability  
Sample:  Standard solution
Suitability requirements  
Tailing factor:  NMT 2.0 for the gabapentin peak
Relative standard deviation:  NMT 5.0% for gabapentin and gabapentin related compound A
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of gabapentin related compound A in the portion of Capsules taken:
Result = ( r U / r S ) × ( C S / C U ) × 100

r U  = = peak response for gabapentin related compound A from the Sample solution  
r S  = = peak response for gabapentin related compound A from the Standard solution  
C S  = = concentration of USP Gabapentin Related Compound A RS in the Standard solution (mg/mL)
C U  = = nominal concentration of gabapentin in the Sample solution (mg/mL)

Calculate the percentage of any other unspecified degradation product, relative to gabapentin content, in the portion of Capsules taken:
Result = ( r U / r S ) × ( C S / C U ) × 100

r U  = = peak response for each unspecified impurity from the Sample solution  
r S  = = peak response for gabapentin from the Standard solution  
C S  = = concentration of USP Gabapentin RS in the Standard solution (mg/mL)
C U  = = nominal concentration of gabapentin in the Sample solution (mg/mL)

Acceptance criteria  
Gabapentin related compound A:  NMT 0.4%
Any individual unspecified impurity:  NMT 0.1%
Total impurities:  NMT 1.0%
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in well-closed containers. Store at controlled room temperature.
•   USP Reference Standards 11
USP Gabapentin RS  
USP Gabapentin Related Compound A RS  
2-Aza-spiro[4.5]decan-3-one.
     C9H15NO          153.22
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph  Heather R. Joyce, Ph.D.
Associate Scientific Liaison
(301) 998-6792  (SM42010) Monographs - Small Molecules 4
711   Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison
(301) 816-8106  (GCDF2010) General Chapters - Dosage Forms
Reference Standards  RS Technical Services
1-301-816-8129
rstech@usp.org   

USP38–NF33 Page 3631
Pharmacopeial Forum: Volume No. 32(6) Page 1693

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