The Column - January 2007 - (Page 25)

Warning : session_start : The session id contains invalid characters, valid characters are only a-z, A-Z and 0-9 in /mnt/data/www.nxtbook.com/fx/config_1.3/global.php on line 9 Warning : session_start : Cannot send session cache limiter - headers already sent output started at /mnt/data/www.nxtbook.com/fx/config_1.3/global.php:9 in /mnt/data/www.nxtbook.com/fx/config_1.3/global.php on line 9 Warning : Cannot modify header information - headers already sent by output started at /mnt/data/www.nxtbook.com/fx/config_1.3/global.php:9 in /mnt/data/www.nxtbook.com/fx/config_1.3/global.php on line 10 January 2007 www.thecolumn.eu.com The Column Marten Demonstration of Chiral Separation Behaviour and a Scale-up Process Silvia Marten, Knauer Scientific Instruments, Berlin, Germany. This article examines the enantioseparation of a racemic cyclic lactone that was performed with a cellulose-based chiral stationary phase. The effects of column temperature and stationary phase particle size on the analytical scale chiral separation were analysed to find the optimal parameters for scaling up the separation process with the highest loadability. Introduction Chiral stationary phases CSPs are made by immobilizing single enantiomers onto a stationary phase. The resolution of any enantioseparation relies on the formation of transient diastereoisomers on the surface of the stationary phase. The forces that lead to this interaction are very weak and require careful optimization by adjustment of the mobile phase and temperature to maximize selectivity. Before performing an enantiomeric separation at the preparative scale, it is highly recommended that analytical scale investigations be performed first. The first step is to find a suitable column material for the chiral separation. In this instance, the polysaccharide-based chiral stationary phase, Eurocel 01, was chosen because of its versatility in polar and non-polar solvents. Based on a wide-pore silica matrix coated with a derivatized cellulose chiral selector tris 3,5dimethylphenylcarbamate Figure 1 , the Eurocel 01 chiral selectors have a propeller-type shape and are believed to form helical polymeric structures that combine polar, - interactions with inclusion complexation. The solubility of the target compound can define the chiral operation mode as well as the required selectivity. The non-polar solvent mixture heptane/2propanol 96:4, v/v was chosen to get a selectivity of more than 1.2 on the analytical column. Author: Silvia Marten E-mail: marten@knauer.net Materials and Methods The following analytical parameters were found to be the most suitable for the normal phase chiral separation of the cyclic lactone racemate: Column: Eurocel 01, 5 µm, 250 4.6 mm i.d. Detection: UV at 215 nm Mobile phase: heptane/2-propanol 96/4, v/v Flow-rate: 1 mL/min Temperature: 10 °C, 20 °C and 45 °C Injection volume: Variable 10–100 µL All analytical analyses were performed with a Knauer Smartline HPLC system equipped with Smartline Pump 1000, Manager 5000, Autosampler 3900, Oven 4000 and UV detector 2600. Results and Discussion The effect of temperature is important on chiral HPLC. Lower temperatures will generally increase chiral recognition, but since they alter the kinetics of mass transfer, they may actually make the chromatography worse by broadening peaks. The chiral separation behaviour of a cyclic lactone was analysed with Eurocel 01 at different temperatures to study this effect. Figure 2 shows an overlay of all three chromatograms at different temperatures. The effect of different temperatures on the enantioseparation is shown in Table 1. In view of these results, 25 Warning : Unknown : The session id contains invalid characters, valid characters are only a-z, A-Z and 0-9 in Unknown on line 0 Warning : Unknown : Failed to write session data files . Please verify that the current setting of session.save_path is correct /var/lib/php/session in Unknown on line 0 http://www.thecolumn.eu.com

Table of Contents for the Digital Edition of The Column - January 2007

Contents
News
Zosimus
Market Trends and Analysis
Extraction of Pharmaceuticals from Environmental Water Samples
Simplified Method Development with a Single Polymeric SPE Sorbent
Chiral Method Development
Demonstration of Chiral Separation Behaviour and a Scale-up Process
Q&A

The Column - January 2007

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