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Use of The Superpure 70 Automated System for Column Loadibility Study for Preparative Chiral Separation of Trans Stilbene Oxide (TSO)
by Anelly Vargas and Harbaksh Sidhu, Thar Technologies, Inc.
The SuperPure 70 System is an automated instrument developed by Thar Technologies for Supercritical Fluid Chromatography (SFC) and HPLC at preparative scale. The system is capable of separating chiral compounds and collecting pure enantiomers, with reliable, fast, and reproducible results (Figure 1).
System Specifications:
operating pressure range with CO2
50 to 200 bar
operating temperature
5 to 80 C at 200 bar
total system flow rate
70 g/min
CO2 flow rate
5 to 70 g/min
co-solvent/modifier flow rate
1 to 50 mL/min
modifier percentage
5 to 100%
fluid/solvent compatibility
CO2 and most organic solvents
max. recommended column size
up to 20 mm i.d. × 500 mm length
sample injection
pump
number of injections
unlimited
sample injection loop
variable
detection
UV
peak collection
three or more independent peaks per injection using cyclone separators
software
Process Suite
Experimental:
We developed a method for the preparative chiral separation of Trans Stilbene Oxide (TSO) using Thar’s SuperPure SFC70 System. Figure 2 shows the results of different loop volumes of 0.5 mL, 1.0 mL, 1.5 mL, and 2.0 mL and their injections under our defined optimal conditions. We used a concentration of TSO (98% purity) in MeOH of 54 mg/mL for 0.5 mL, 1.5 mL, and 2.0 mL. We also used 73% pure TSO with the cis impurity for the 1.0-mL loop at the same concentration.
SFC enantiomer separation using column: CHIRACEL OD® (i.d. 20 mm × 500 mm length, adsorbent: cellulose tris)
Supercritical CO2 + 8.2% MeOH as mobile phase
Flow 58.8 g/min
Column and CO2 temperature 60 C respectively
BPR 100 bar
Pressure drop 34 bar
Sample concentration 54 mg TSO/mL in MeOH
Figure 1: SuperPure SFC70 system.
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Results:
Significantly, we found that the column loadability and loop effect study at different loop sizes and purity of the compound show minimal change in retention time. Therefore, we were able to increase the loop size by a factor of four and achieve good separation for collection thereby increasing our productivity.
Figure 2: Chromatogram of TSO SFC70
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Thar Technologies, Inc.
100 Beta Drive
Pittsburgh, PA 15238
phenylamine, should be included in the mix. Similarly, derivative azobenzene should be included in the mix, in place of unstable target compound diphenylhydrazine.
For identification of all peaks, request Restek Advantage newsletter 2004v2 (lit.# 59037) or see www.restek.com
Figure 1. 15-minute separation of US EPA Method 8270D semivolatile organics on a 20 m × 0.18 mm ID column.
Column: Rtx®-5 Sil MS, 20 m, 0.18 mm ID, 0.18 μm df (cat.# 42702); Sample: 8270 MegaMix™ 76-component calibration mix (cat.# 31686), benzoic acid (31415), benzidine (31441), 2,4-dinitrophenol (31291), Acid Surrogate Mix (31063), B/N Surrogate Mix (31062), SV Internal Standard Mix (31206), 0.5 μL, 5 ppm each compound / 2.5 ng on column (2,4-dinitrophenol: 10 ppm/5 ng; 3-, 4- methylphenol: 2.5 ppm/1.25 ng each, for calibration at lower levels and quantification at required limits); Injection: splitless, hold 0.15 min., pressure pulse 0.20 min. @ 30 psi, 2 mm ID cyclo double gooseneck inlet liner (cat.# 20907), 270 C; Instrument: Agilent 6890/5973 GC/MS; Carrier Gas: helium, 1.2 mL/min., constant flow; Oven Temp.: 40 C (hold 0.5 min.) to 90 C @ 14 C/min., to 330 C @ 22 C/min. (hold 1 min.); Transfer Line Temp.: 280 C; Scan Range: 35 to 550 amu; Solvent Delay: 1 min.; Tune: DFTPP; Ionization: EI. GC_EV00736 Peaks: 1) N-nitrosodimethylamine, 2) pyridine, 4) aniline, 6) phenol, 50) 2,4-dinitrophenol, 66) pentachlorophenol, 83) benzo(b)fluoranthene, 84) benzo(k)fluoranthene.
Restek Corp.
110 Benner Circle
Bellefonte, PA 16823-8812
Thar Instruments, Inc.
575 Epsilon Dr., Suite 100
Pittsburgh, PA, 15238
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