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小木虫论坛-学术科研互动平台 » 生物医药区 » 新药研发 » 质量控制 » 【求助】英国药典阿奇霉素质量标准
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ccmaodou

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[交流] 【求助】英国药典阿奇霉素质量标准已有6人参与

英国药典阿奇霉素质量标准！

先谢谢了！
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1楼2010-04-15 22:45:27
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jgy2000

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ccmaodou(金币+1):谢谢参与
ccmaodou(金币+17): 2010-04-18 12:27
www.drugfuture.com网上有美国、英国、日本药典全文，全是最新的
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6楼2010-04-16 23:35:08
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jinyixiao

至尊木虫 (著名写手)
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ccmaodou(金币+1):谢谢参与
ccmaodou(金币+20):十分感谢！ 2010-04-16 08:17
(Ph Eur monograph 1649)
  


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C38H72N2O12   749   83905-01-5
  
Action and use
  
Antibacterial.
  
Ph Eur
  
  
DEFINITION
  
(2R,3S,4R,5R,8R,10R,11R,12S,13S,14R)-13-[(2,6-Dideoxy-3-C-methyl-3-O-methyl-a-L-ribo-hexopyranosyl)oxy]-2-ethyl-3,4,10-trihydroxy-3,5,6,8,10,12,14-heptamethyl-11-[[3,4,6-trideoxy-3-(dimethylamino)-b-D-xylo-hexopyranosyl]oxy]-1-oxa-6- azacyclopentadecan-15-one.
  
Content
  
94.0 per cent to 102.0 per cent (anhydrous substance).
  
CHARACTERS
  
Appearance
  
White or almost white powder.
  
Solubility
  
Practically insoluble in water, freely soluble in anhydrous ethanol and in methylene  chloride.
  
IDENTIFICATION
  
 A. Infrared absorption spectrophotometry (2.2.24).
  
Comparison azithromycin CRS.
  
If the spectra obtained in the solid state show differences, prepare further spectra  using 90 g/l solutions in methylene chloride R.
  
 B. Examine the chromatograms obtained in the assay.
  
Results The principal peak in the chromatogram obtained with test solution (b) is  similar in retention time and size to the principal peak in the chromatogram obtained  with reference solution (a).
  
TESTS
  
Solution S
  
Dissolve 0.500 g in anhydrous ethanol R and dilute to 50.0 ml with the same solvent.
  
Appearance of solution
  
Solution S is clear (2.2.1) and colourless (2.2.2, Method II).
  
pH (2.2.3)
  
9.0 to 11.0.
  
Dissolve 0.100 g in 25.0 ml of methanol R and dilute to 50.0 ml with carbon dioxide-free water R.
  
Specific optical rotation (2.2.7)
  
  - 45 to - 49 (anhydrous substance), determined on solution S.
  
Related substances
  
Liquid chromatography (2.2.29). Prepare the solutions immediately before use.
  
Solvent mixture acetonitrile R, water R (40:60 V/V).
  
Test solution (a) Dissolve 0.100 g of the substance to be examined in the solvent  mixture and dilute to 25.0 ml with the solvent mixture.
  
Test solution (b) Dilute 5.0 ml of test solution (a) to 20.0 ml with the solvent  mixture.
  
Reference solution (a) Dissolve 50.0 mg of azithromycin CRS in the solvent mixture  and dilute to 50.0 ml with the solvent mixture.
  
Reference solution (b) Dilute 1.0 ml of test solution (a) to 100.0 ml with the solvent  mixture.
  
Reference solution (c) Dissolve 5.0 mg of azithromycin CRS and 5.0 mg of  azithromycin impurity A CRS in the solvent mixture and dilute to 50 ml with the  solvent mixture.
  
Reference solution (d) Dissolve the contents of a vial of azithromycin impurity B  CRS in 1.0 ml of the solvent mixture. Use this solution for identification of the peak  due to impurity B.
  
Column: 
 —size: l = 0.25 m, Ø = 4.6 mm,
  
 —stationary phase: end-capped polar-embedded octadecylsilyl amorphous organosilica polymer R (5 µm),
  
 —temperature: 70 °C.
  
Mobile phase Mix 10 volumes of a 34.84 g/l solution of dipotassium hydrogen  phosphate R previously adjusted to pH 6.5 with phosphoric acid R, 35 volumes of  acetonitrile R and 55 volumes of water R.
  
Flow rate 1.0 ml/min.
  
Detection Spectrophotometer at 215 nm.
  
Injection 100 µl of test solution (a) and reference solutions (b), (c) and (d).
  
Run time 4.5 times the retention time of azithromycin.
  
Relative retention With reference to azithromycin (retention time = about 26 min):  impurity D = about 0.37; impurity J = about 0.39; impurity A = about 0.42; impurity I  = about 0.5; impurity C = about 0.65; impurity K = about 0.9; impurity F = about 1.6;  impurity B = about 1.7; impurity G = about 2.8.
  
System suitability Reference solution (c):
  
 —resolution: minimum 7.0 between the peaks due to impurity A and azithromycin.
  
Limits:  
 —impurity B: not more than twice the area of the principal peak in the chromatogram obtained with reference solution (b) (2.0 per cent),
  
 —any other impurity: for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (1.0 per cent),
  
 —total: not more than 5 times the area of the principal peak in the chromatogram obtained with reference solution (b) (5.0 per cent),
  
 —disregard limit: 0.1 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.1 per cent).
  
  
Heavy metals (2.4.8)
  
Maximum 25 ppm.
  
Dissolve 2.0 g in a mixture of 15 volumes of water R and 85 volumes of anhydrous  ethanol R and dilute to 20 ml with the same mixture of solvents. 12 ml of the solution  complies with test B. Prepare the reference solution using lead standard solution  (2.5 ppm Pb) obtained by diluting lead standard solution (100 ppm Pb) R with a  mixture of 15 volumes of water R and 85 volumes of anhydrous ethanol R.
  
Water (2.5.12)
  
1.8 per cent to 6.5 per cent, determined on 0.200 g.
  
Sulphated ash (2.4.14)
  
Maximum 0.2 per cent, determined on 1.0 g.
  
ASSAY
  
Liquid chromatography (2.2.29) as described in the test for related substances, with  the following modification.  
  
Injection 25 µl of test solution (b) and reference solution (a).
  
Calculate the percentage content of C38H72N2O12 using the declared content of  azithromycin CRS.
  
STORAGE
  
In an airtight container .
  
IMPURITIES
  
Specified impurities A, B, C, D, E, F, G, H, I, J, K.
  


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 A. R1 = OH, R2 = H, R3 = R4 = R5 = CH3: 6-demethylazithromycin,
  
 B. R1 = H, R2 = R3 = R4 = R5 = CH3: 3-deoxyazithromycin (azithromycin B),
  
 C. R1 = OH, R2 = R3 = R5 = CH3, R4 = H: 3¢-O-demethylazithromycin (azithromycin C),
  
 D. R1 = OH, R2 = R3 = R4 = CH3, R5 = CH2OH: 14-demethyl-14-(hydroxymethyl)azithromycin (azithromycin F),
  
 F. R1 = OH, R2 = R4 = R5 = CH3, R3 = CHO: 3¢-N-demethyl-3¢-N-formylazithromycin,
  
 G. R1 = OH, R2 = R4 = R5 = CH3, R3 = SO2-C6H4-CH3: 3¢-N-demethyl-3¢-N-[(4-methylphenyl)sulphonyl]azithromycin,
  
 I. R1 = OH, R2 = R4 = R5 = CH3, R3 = H: 3¢-N-demethylazithromycin,
  


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 E. 3¢-(N,N-didemethyl)azithromycin (aminoazithromycin),
  


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 H. 3¢-de(dimethylamino)-3¢,4¢-didehydroazithromycin,
  


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 J. decladinosylazithromycin,
  


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 K. (2S,4¢R,4aR,5¢S,6¢S,7R,8S,9R,10R,13R,15R,16R,17S,17aS)-7-ethyl-5¢,8,9,15-tetrahydroxy-4¢-methoxy-4¢,6¢,8,10,11,13,15,17-octamethyl-16-[[3,4,6-trideoxy-3-(dimethylamino)-b-D-xylo-hexopyranosyl]oxy]octadecahydro-5H-spiro[1,3-dioxino[4,5-m][1,6]oxazacyclopentadecine-2,2¢-[2H]pyran]-5-one (azithromycin E).
  

  Ph Eur
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2楼2010-04-15 22:54:08
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jinyixiao

至尊木虫 (著名写手)
上面是英国药典（2007）上面的相关内容。其中一些分子结构式显示不出。
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3楼2010-04-15 22:56:51
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mrzouhao

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ccmaodou(金币+1):谢谢参与
ccmaodou(金币+10): 2010-04-16 09:21
http://www.newdruginfo.com/ypbz/bzjs/aqms.htm
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4楼2010-04-16 08:08:46
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