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小木虫论坛-学术科研互动平台 » 生物医药区 » 药学 » 药典 » Vinblastine Sulfate 和 Capecitabine 的usp35标准
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kebog

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[求助] Vinblastine Sulfate 和 Capecitabine 的usp35标准

各位大虾：
求助 Vinblastine Sulfate 和 Capecitabine   这两个原料药的usp35标准
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1楼2012-07-08 14:47:45
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xiaoxiao270: 金币+1, 3Q 2012-07-08 19:06:35
只找到USP32的
Vinblastine Sulfate

http://db.yaozh.com/foreign/USP2 ... stine%20Sulfate.htm

Capecitabine
http://db.yaozh.com/foreign/usp32/v32270/Capecitabine.html
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2楼2012-07-08 16:03:44
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Tadalafil

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kebog: 金币+1, ★★★★★最佳答案, 非常感谢！也麻烦提供Capecitabine 的usp35标准。 2012-07-08 22:59:30
Vinblastine Sulfate USP35
Vinblastine Sulfate
(vin blas' teen sul' fate).
  

C46H58N4O9·H2SO4 909.05
Vincaleukoblastine, sulfate (1:1) (salt);     
Vincaleukoblastine sulfate (1:1) (salt)     [143-67-9].
DEFINITION
Vinblastine Sulfate contains NLT 96.0% and NMT 102.0% of C46H58N4O9·H2SO4, corrections being applied for loss in weight.
[Caution—Handle Vinblastine Sulfate with great care, because it is a potent cytotoxic agent. ]
IDENTIFICATION
•  A. Infrared Absorption 197K
Analysis:  The sample specimen and reference standard are previously dried in vacuum at 60 for 16 h.
Acceptance criteria:  Meets the requirements
•  B. Identification Tests—General, Sulfate 191
Sample:  100 mg/mL in water
Acceptance criteria:  Meets the requirements
ASSAY
Change to read:
•  Procedure
Solution A:  Diethylamine and water (14:986). Adjust with phosphoric acid to a pH of 7.5.
Solution B:  Acetonitrile and methanol (20:80)
Mobile phase:  Solution A and Solution B (38:62)
Standard solution:  0.4 mg/mL of USP Vinblastine Sulfate RS in water
System suitability solution:  0.4 mg/mL each of vincristine sulfate and vinblastine sulfate in water prepared as follows. Transfer USP Vincristine Sulfate RS or USP Vincristine Sulfate (Assay) RS(RB 1-Jul-2011) to a suitable volumetric flask, and dissolve in the Standard solution.
Sample solution:  0.4 mg/mL of Vinblastine Sulfate in water
Chromatographic system  
(See Chromatography 621, System Suitability.)
Mode:  LC
Detector:  UV 262 nm
Columns  
Precolumn:  Packed with porous silica gel; installed between the pump and the injector
Analytical:  4.6-mm × 15-cm; packing L1
Flow rate:  2 mL/min
Injection size:  20 µL
System suitability  
Samples:  Standard solution and System suitability solution
Suitability requirements  
Resolution:  NLT 4.0 between vincristine and vinblastine, System suitability solution
Relative standard deviation:  NMT 2.0%, Standard solution
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of vinblastine sulfate (C46H58N4O9·H2SO4) in the portion of Vinblastine Sulfate 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 Vinblastine Sulfate RS in the Standard solution (mg/mL)
CU = = concentration of Vinblastine Sulfate in the Sample solution (mg/mL)

Acceptance criteria:  96.0%–102.0%, corrections being applied for loss in weight
IMPURITIES
•  Organic Impurities
Mobile phase, System suitability solution, and System suitability:  Proceed as directed in the Assay.
Sample solution A:  Use the Sample solution prepared in the Assay.
Sample solution B:  16 µg/mL of vinblastine sulfate in water from Sample solution A
Chromatographic system  
(See Chromatography 621, System Suitability.)
Mode:  LC
Detector:  UV 262 nm
Columns  
Precolumn:  Packed with porous silica gel; installed between the pump and the injector
Analytical:  4.6-mm × 15-cm; packing L1
Flow rate:  2 mL/min
Injection size:  200 µL
Analysis  
Samples:  Sample solution A and Sample solution B
Calculate the percentage of each individual impurity in the portion of Vinblastine Sulfate taken:
Result = [rUA/(SrUA + 25rUB)] × 100
rUA = = peak response for each individual impurity appearing after the solvent peak from Sample solution A
rUB = = peak response for vinblastine from Sample solution B

Calculate the percentage of total impurities:
Result = [(SrUA/(SrUA + 25rUB)] × 100
rUA = = peak response for each impurity appearing after the solvent peak from Sample solution A
rUB = = peak response for vinblastine from Sample solution B

Acceptance criteria  
Individual impurities:  NMT 1.0%
Total impurities:  NMT 3.0%
SPECIFIC TESTS
•  pH 791
Sample:  1.5 mg/mL in water
Acceptance criteria:  3.5–5.0
•  Loss on Drying
(See Thermal Analysis 891.)
[Note—In this procedure, perform weighings rapidly with minimum exposure of the substances to air. ]
Sample:  10 mg
Analysis:  Determine the percentage of volatile substances by thermogravimetric analysis on an appropriately calibrated instrument. Heat the Sample at the rate of 5/min between ambient temperature and 200 in an atmosphere of nitrogen at a flow rate of 40 mL/min. From the thermogram, determine the accumulated loss in weight between ambient temperature and a point on the plateau before decomposition is indicated (about 160).
Acceptance criteria:  It loses NMT 15.0% of its weight.
•  Sterility Tests 71: Where the label states that Vinblastine Sulfate is sterile, it meets the requirements.
•  Bacterial Endotoxins Test 85: Where the label states that Vinblastine Sulfate is sterile or must be subjected to further processing during the preparation of injectable dosage forms, it contains NMT 10.0 USP Endotoxin Units/mg of vinblastine sulfate.
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in tight, light-resistant containers, and store in a freezer.
•  Labeling: Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
Change to read:
•  USP Reference Standards 11
USP Endotoxin RS
USP Vinblastine Sulfate RS  
USP Vincristine Sulfate RS  
[Note—No loss on drying determination is needed. ]
USP Vincristine Sulfate (Assay) RS
(RB 1-Jul-2011)
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Feiwen Mao, M.S.
Senior Scientific Liaison
1-301-816-8320 (SM32010) Monographs - Small Molecules 3
71 Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison
1-301-816-8339 (GCM2010) General Chapters - Microbiology
85 Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison
1-301-816-8339 (GCM2010) General Chapters - Microbiology
Reference Standards RS Technical Services
1-301-816-8129
rstech@usp.org  

USP35–NF30 Page 5020
USP35–NF30 Supplement : No. 1 Page 5117
Pharmacopeial Forum: Volume No. 32(5) Page 1470
Chromatographic Column—  
VINBLASTINE SULFATE
Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30.
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3楼2012-07-08 22:45:45
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Tadalafil

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kebog: 金币+1, ★★★★★最佳答案, 非常感谢！ 2012-07-08 23:13:31
Capecitabine USP35
Capecitabine
(kap'' e sye' ta been).
  

C15H22FN3O6 359.35
Carbamic acid, [1-(5-deoxy--d-ribofuranosyl)-5-fluoro-1,2-dihydro-2-oxo-4-pyrimidinyl]-, pentyl ester;     
Pentyl 1-(5-deoxy--d-ribofuranosyl)-5-fluoro-1,2-dihydro-2-oxo-4-pyrimidinecarbamate     [154361-50-9].
DEFINITION
Capecitabine contains NLT 98.0% and NMT 102.0% of C15H22FN3O6, calculated on the anhydrous and solvent-free basis.
IDENTIFICATION
•  A. Infrared Absorption 197K
Sample:  2 mg of sample in 300 mg of potassium bromide
•  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:  Methanol, acetonitrile, and water (7:1:12)
Solution A:  0.1% mixture of glacial acetic acid in water
Solution B:  Methanol, acetonitrile, and Solution A (7:1:12)
Solution C:  Methanol, acetonitrile, and Solution A (16:1:3)
Mobile phase:  See the gradient table below.
Time
(min) Solution B
(%) Solution C
(%)
0 100 0
5 100 0
20 49 51
30 49 51
31 100 0
40 100 0

[Note—The following solutions may be sonicated if necessary. ]
System suitability solution:  0.6 µg/mL each of USP Capecitabine RS, USP Capecitabine Related Compound A RS, USP Capecitabine Related Compound B RS, and USP Capecitabine Related Compound C RS in Diluent
Standard solution:  0.6 mg/mL of USP Capecitabine RS in Diluent
Sample solution:  0.6 mg/mL of Capecitabine in Diluent
Chromatographic system  
(See Chromatography 621, System Suitability.)
Mode:  LC
Detector:  UV 250 nm
Column:  4.6-mm × 25-cm; 5-µm packing L1
Column temperature:  40
Autosampler temperature:  5
Flow rate:  1 mL/min
Injection size:  10 µL
System suitability  
Samples:  System suitability solution and Standard solution
[Note—For the purpose of peak identification, the approximate relative retention times are given in Impurity Table 1. The relative retention times are measured with respect to capecitabine. ]
Suitability requirements  
Resolution:  NLT 1.0 between capecitabine related compound A and capecitabine related compound B, System suitability solution
Tailing factor:  NMT 1.5, Standard solution
Relative standard deviation:  NMT 2.0%, Standard solution
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of C15H22FN3O6 in the portion of Capecitabine 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 Capecitabine RS in the Standard solution (mg/mL)
CU = = concentration of Capecitabine in the Sample solution (mg/mL)

Acceptance criteria:  98.0%–102.0% on the anhydrous and solvent-free basis
IMPURITIES
Inorganic Impurities  
•  Residue on Ignition 281: NMT 0.1%
•  Heavy Metals, Method II 231: NMT 20 ppm
Organic Impurities  
•  Procedure
Diluent, Solution B, Solution C, System suitability solution, Standard solution, Sample solution, and Chromatographic system:  Proceed as directed in the Assay.
Analysis  
Samples:  Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Capecitabine taken:
Result = (rU/rS) × (CS/CU) × 100/F
rU = = peak response for each impurity from the Sample solution
rS = = peak response for capecitabine from the Standard solution
CS = = concentration of USP Capecitabine RS in the Standard solution (mg/mL)
CU = = concentration of Capecitabine in the Sample solution (mg/mL)
F = = relative response factor for an impurity, from Impurity Table 1  

Acceptance criteria  
Individual impurities:  See Impurity Table 1.
Total impurities:  NMT 1.5%
Impurity Table 1
Name Relative
Retention
Time Relative
Response
Factor  Acceptance
Criteria,
NMT (%)
Capecitabine related compound A 0.18 1.05 0.3
Capecitabine related compound B 0.19 0.81 0.3
2¢,3¢-Di-O-acetyl-5¢-deoxy-5-fluorocytidine 0.36 0.89 0.1
5¢-Deoxy-5-fluoro-N4-(2-methyl-1-butyloxycarbonyl)cytidine + 5¢-Deoxy-5-fluoro-N4-(3-methyl-1-butyloxycarbonyl)cytidine 0.95 1.01 0.5
Capecitabine 1.00 1.00 —
[1-[5-Deoxy-3-O-(5-deoxy--d-ribofuranosyl)--d-ribofuranosyl]-5-fluoro-2-oxo-1,2-dihydropyrimidin-4-yl]-carbamic acid pentyl ester 1.06 1.00 0.3
[1-[5-Deoxy-2-O-(5-deoxy--d-ribofuranosyl)--d-ribofuranosyl]-5-fluoro-2-oxo-1,2-dihydropyrimidin-4-yl]-carbamic acid pentyl ester 1.09 1.00 0.2
Capecitabine related compound C 1.11 0.91 0.3
[1-[5-Deoxy-3-O-(5-deoxy--d-ribofuranosyl)--d-ribofuranosyl]-5-fluoro-2-oxo-1,2-dihydropyrimidin-4-yl]-carbamic acid pentyl ester 1.20 1.00 0.3
2¢,3¢-Di-O-acetyl-5¢-deoxy-5-fluoro-N4-(pentyloxycarbonyl)cytidine 1.37 0.85 0.1
Individual unspecified impurity — 1.00 0.1

SPECIFIC TESTS
•  Optical Rotation, Specific Rotation 781S: +96.0 to +100.0
Sample solution:  10 mg/mL, on the anhydrous and solvent-free basis, in methanol, at 20
•  Water Determination, Method Ic 921: NMT 0.3%
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in tight containers. Store at controlled room temperature.
•  USP Reference Standards 11
USP Capecitabine RS  
USP Capecitabine Related Compound A RS  
5¢-Deoxy-5-fluorocytidine.
    C9H12FN3O4        245.21
USP Capecitabine Related Compound B RS  
5¢-Deoxy-5-fluorouridine.
    C9H11FN2O5        246.19
USP Capecitabine Related Compound C RS  
2¢,3¢-O-Carbonyl-5¢-deoxy-5-fluoro-N4-(pentyloxycarbonyl)cytidine.
    C16H20FN3O7        385.34
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Feiwen Mao, M.S.
Senior Scientific Liaison
1-301-816-8320 (SM32010) Monographs - Small Molecules 3
Reference Standards RS Technical Services
1-301-816-8129
rstech@usp.org  

USP35–NF30 Page 2469
Pharmacopeial Forum: Volume No. 35(4) Page 834
Chromatographic Column—  
CAPECITABINE
Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30.



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4楼2012-07-08 22:47:57
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Tadalafil

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Capecitabine见4楼
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5楼2012-07-08 23:01:02
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kebog

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引用回帖:
4楼: Originally posted by Tadalafil at 2012-07-08 22:47:57
Capecitabine USP35
Capecitabine
(kap'' e sye' ta been).
  

C15H22FN3O6 359.35
Carbamic acid, -, pentyl ester;     
Pentyl 1-(5-deoxy--d-ribofuranosyl)-5-fluoro-1,2-dihydro-2-oxo-4-pyrimid ...

麻烦提供pdf版，邮箱：wangmm666@163.com   谢谢！如果两个都有pdf版，请都提供，谢谢啦！
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6楼2012-07-08 23:04:12
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Tadalafil

银虫 (小有名气)

【答案】应助回帖

引用回帖:
6楼: Originally posted by kebog at 2012-07-08 23:04:12
麻烦提供pdf版，邮箱：wangmm666@163.com   谢谢！如果两个都有pdf版，请都提供，谢谢啦！...

已发送，请查收

两个都是pdf版。版本：USP 35–NF 30 through Second Supplement
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7楼2012-07-08 23:10:21
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