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qiuqinglei5020

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[求助] 阿哌沙班液相分析条件？

有做阿哌沙班的吗？液相条件帮忙说一下

回复此楼

1楼 2013-10-17 15:20:06

已阅回复此楼关注TA 给TA发消息送TA红花 TA的回帖

yanghuping

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【答案】应助回帖

感谢参与，应助指数 +1

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.