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Ò©µä·½·¨ÇóÖú ¸÷λÀÏʦ£¬°ï°ïæ¡£ÒÔÏÂÊÇÒ©µä·½·¨£º Silylation solution. To 2 mL of N,O-bis(trimethylsilyl)tri- fluoroacetamide R add 0.04 mL of chlorotrimethylsilane R and mix. Test solution.Dissolve50.0mgofthesubstancetobeexamined in 3 mL of water R and add 0.5 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylenechlorideR. Evaporate the combined methylene chloride extracts to dryness in a vial with a screw cap and add 0.5 mL of the silylation solution.Sealthevialandheatat70¡À5¡ãCfor20min. ÆäÖУ¬Seal the vial and heat at 70¡À5¡ãC for 20min.Õâ¸öÊǵ¥µ¥Ö¸¹èÍ黯·´Ó¦µÄζȺÍʱ¼äÂð£¿ÓÐûÓаüÀ¨ºóÃæ¶¥¿ÕƽºâµÄζȺÍʱ¼ä£¿»¹ÊÇ˵ºóÃæ¶¥¿ÕƽºâµÄζȺÍʱ¼äÐèÒª×Ô¼ºÃþË÷É趨? |
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ltxin2009
Ìú¸Ëľ³æ (Ö°Òµ×÷¼Ò)
- ACI: 1
- Ó¦Öú: 157 (¸ßÖÐÉú)
- ¹ó±ö: 0.368
- ½ð±Ò: 6510.3
- É¢½ð: 1025
- ºì»¨: 29
- ɳ·¢: 1
- Ìû×Ó: 3711
- ÔÚÏß: 1610.3Сʱ
- ³æºÅ: 1100553
- ×¢²á: 2010-09-16
- ÐÔ±ð: GG
- רҵ: É«Æ×·ÖÎö
2Â¥2012-02-07 12:00:46
yzhlasiI
Ìú³æ (ÕýʽдÊÖ)
- Ó¦Öú: 4 (Ó×¶ùÔ°)
- ½ð±Ò: 28.3
- É¢½ð: 6
- Ìû×Ó: 392
- ÔÚÏß: 57.3Сʱ
- ³æºÅ: 1217620
- ×¢²á: 2011-03-01
|
ÕâÊÇÕû¸öÆøÏà·½·¨£º TESTS pH (2.2.3): 6.5 to 7.5. Dissolve 0.20 g in carbon dioxide-free water R and dilute to 10 mL with the same solvent. Impurity C. Gas chromatography (2.2.28). Silylation solution. To 2 mL of N,O-bis(trimethylsilyl)tri- fluoroacetamide R add 0.04 mL of chlorotrimethylsilane R and mix. Test solution.Dissolve50.0mgofthesubstancetobeexamined in 3 mL of water R and add 0.5 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylenechlorideR. Evaporate the combined methylene chloride extracts to dryness in a vial with a screw cap and add 0.5 mL of the silylation solution.Sealthevialandheatat70¡À5¡ãCfor20min. Reference solution (a).Dissolve5.0mgof sodium phenylbutyrate impurity C CRS in methylenechlorideR and dilute to 10.0 mL with the same solvent. Reference solution (b). Dilute 1.0 mL of reference solution (a) to 10.0 mL with methylenechlorideR.Place1.0mLofthis solution in a vial with a screw cap, evaporate to dryness and add 0.5 mL of the silylation solution. Seal the vial and heat at 70¡À5¡ãCfor20min. Reference solution (c). Dissolve 10 mg of the substance to be examined in 25 mL of water R. To 3 mL of this solution add 0.1 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylene chloride R. Combine the methylene chloride extracts in a vial with a screw cap and add 2 mL of reference solution (a). Evaporate to dryness and add 0.5 mL of the silylation solution. Seal the vial and heat at 70 ¡À 5 ¡ãC for 20 min. Column: ¡ª material :fusedsilica; ¡ª size: l =25m,Ø=0.25mm; ¡ª stationary phase: poly(dimethyl)(diphenyl)siloxane R (film thickness 1.0 ¦Ìm). Carrier gas : helium for chromatography R. Flow rate:0.9mL/min. Split ratio: 1:100. Temperature: Time(min) Temperature(¡ãC) Column 0-5 50 5 - 27 50 ¡ú 270 27 ¨C 32 270 Injection port 270 Detector 270 Detection:flameionisation. Injection:1 ¦ÌL. Relative retention with reference to phenylbutyrate (retention time = about 20 min) : impurity C = about 0.98. System suitability: reference solution (c) : ¡ª resolution: minimum 3.0 between the peaks due to impurity C and phenylbutyrate. Limit : ¡ª impurity C:notmorethantheareaofthecorresponding peak in the chromatogram obtained with reference solution (b) (0.1 per cent). Related substances. Liquid chromatography (2.2.29). |
3Â¥2012-02-07 16:07:41
ltxin2009
Ìú¸Ëľ³æ (Ö°Òµ×÷¼Ò)
- ACI: 1
- Ó¦Öú: 157 (¸ßÖÐÉú)
- ¹ó±ö: 0.368
- ½ð±Ò: 6510.3
- É¢½ð: 1025
- ºì»¨: 29
- ɳ·¢: 1
- Ìû×Ó: 3711
- ÔÚÏß: 1610.3Сʱ
- ³æºÅ: 1100553
- ×¢²á: 2010-09-16
- ÐÔ±ð: GG
- רҵ: É«Æ×·ÖÎö
4Â¥2012-02-07 16:17:25














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