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qiuqinglei5020
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[求助]
阿哌沙班液相分析条件？
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| 有做阿哌沙班的吗？液相条件帮忙说一下 |
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有一篇文献上面的分析条件：General Experimental: All reagents used were of ACS grade or higher. Flash chromatography was performed using either a Biotage Flash Chromatography System or an AnaLogix BSR Solvent Pump System with silica gel cartridges. HPLC analyses for the syntheses were performed on an Agilent 1100 HPLC system including solvent degasser, pump, automated injector and variable UV detector connected to either an IN/US BetaRam Flow Detector with a 0.25ml detector cell or a Berthold Scintillation Detector with a 0.5 ml detector cell. HPLC gradient 1 = Phenomenex Luna C18, 5 mm, 4.6150mm column. Mobile phase A = 0.05% TFA in water, mobile phase B = 0.05% TFA in acetonitrile, 0min 95% A, 6min 50% A, 11 min 95% B, 13 min 95% B, 15 min 95% A, UV detection at 254 nm. HPLC gradient 2 = Vydac protein and peptide C18, 4.6250mm column. Mobile phase A= 0.05% TFA in water, mobile phase B = 0.05% TFA in acetonitrile, 0min 90% A, 16 min 90% B, 23 min 95% B, 25 min 90% A, UV detection at 254 nm. HPLC Gradient 3 = Phenomenex, Luna, C18 (2), 3 mm, 1504.6mm column with Brownlee, RP-18 C18, 3 mm, 153.2mm guard column, column temperature = 301C, autosampler temperature = 41C, mobile phase A = 0.4% formic acid in water adjusted to pH 3.2 with NH4OH, mobile phase B = acetonitrile, mobile phase C = MeOH, 0 min 100% A, 25 min 20% A and 80% B, 27min 50% B and 50% C, 32 min 50% B and 50% C, 34 min 100% A, flowrate = 1.0ml/min at 323 nm. HPLC Gradient 4 =Ace 3, C18, 3 mm, 1504.6mm column with Ace 3, C18, 3 mm, 103.0mm guard column, column temperature = 351C, autosampler temperature = ambient, mobile phase A = 0.4% formic acid in water, adjusted to pH 3.2 with NH4OH, mobile phase B = acetonitrile, 0min 100% A, 3min 100% A, 5min 90% A, 20 min 75% A, 50 min 75% A, 60 min 50% A, 65 min 100% B, 70 min 100% B, 72 min 100% A, flowrate = 0.7ml/min, UV detection at 240 nm. Preparative HPLC condition 1: Phenomenex Luna 5 mm, 25021.2mm column. Mobile phase A = 0.1% TFA in water, mobile phase B = 0.1% TFA in acetonitrile, 0 min 70% A, 18 min 95% B, 22 min 95% B, 25 min 70% A, flowrate = 15 ml/min. UV detection at 254 nm. Preparative HPLC condition 2: Zorbax SB-C18 5 mm, 25021.2mm column. Mobile phase A = 0.05% TFA in water, mobile phase B = 0.05% TFA in acetonitrile, 0 min 90% A, 16 min 90% B, 23 min 95% B, 25 min 90% A, Flowrate = 9.9ml/min, UV detection at 254 nm. LC/MS analysis was performed on a Finnigan LXQ Mass Spectrometer System. NMR spectra were recorded on a Bruker AVANCE II 300MHz Spectrometer with an UltrashieldTM Magnet or a Varian Unity/Inova 300MHz Spectrometer. Specific activities were performed gravimetrically. Liquid scintillation counting was performed on either a PerkinElmer Tri-Carb Model 2900Tr or a Wallac Model 1409 Liquid Scintillation Counter. |
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2013-10-17 15:46:21, 998.45 K
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