Column supercritical fluid chromatography

T. A. Berger, Practical advantages of packed column supercritical fluid chromatography in supporting combinations chemistiy , in Unified Chromatography, J. P. Parcher and T. L. Chester (Eds), ACS Symposium Series 748, American Chemical Society, Washington, DC, pp. 203-233 (2000). 

T. L. Chester and J. D. Pinkston, Pressure-regulating fluid interface and phase behavior considerations in the coupling of packed-column supercritical fluid chromatography with low-pressure detectors , ]. Chromatogr. 807 265-273 (1998). 

Figure 12.23 SFC-SFC analysis, involving a rotaiy valve interface, of a standard coal tar sample (SRM 1597). Two fractions were collected from the first SFC separation (a) and then analyzed simultaneously in the second SFC system (h) cuts a and h are taken between 20.2 and 21.2 min, and 38.7 and 40.2 min, respectively. Peak identification is as follows 1, tii-phenylene 2, chrysene 3, henzo[g/ i]perylene 4, antliracene. Reprinted from Analytical Chemistry, 62, Z. Juvancz et al, Multidimensional packed capillary coupled to open tubular column supercritical fluid chromatography using a valve-switcliing interface , pp. 1384-1388, copyright 1990, with permission from the American Chemical Society.

Figure 12.24 Schematic diagram of the multidimensional packed capillary to open tubular column SFC-SFC system. Reprinted from Analytical Chemistry, 62, Z. Juvancz et al., Multidimensional packed capillary coupled to open tubular column supercritical fluid chromatography using a valve-switching interface , pp. 1384-1388, copyright 1990, with permission from the American Chemical Society.

A number of analytical techniques such as FTIR spectroscopy,65-66 13C NMR,67,68 solid-state 13 C NMR,69 GPC or size exclusion chromatography (SEC),67-72 HPLC,73 mass spectrometric analysis,74 differential scanning calorimetry (DSC),67 75 76 and dynamic mechanical analysis (DMA)77 78 have been utilized to characterize resole syntheses and crosslinking reactions. Packed-column supercritical fluid chromatography with a negative-ion atmospheric pressure chemical ionization mass spectrometric detector has also been used to separate and characterize resoles resins.79 This section provides some examples of how these techniques are used in practical applications. 

Buskov, S., Sprensen, H., and Sprensen, S., Separation of chlorophylls and their degradation products using packed column supercritical fluid chromatography (SEC), J. High Resol. Chromatogr, 22, 339, 1999. 

INFLUENCE OF COLUMN INTERNAL DIAMETER ON EFFICIENCY AMD SEPARATION TIME FOR OPEN TUBUALR COLUMN SUPERCRITICAL FLUID CHROMATOGRAPHY. 

Packed columns, 10 769-772, 773 band broadening, 6 412 for distillzation, 5 768-776 gas chromatography, 6 377, 379 instrumentation, 6 423-424 Packed column supercritical fluid chromatography (pSFC), 19 567 Packed fiber-bed mist eliminators, 23 781 Packed towers, 25 810, 811 Packing(s)... 

Klesper, E. Corwin, A. H. Turner, D. A. J. Org. Chem., 1962, 27, 700. Sugiyama, K. Saito, M. Hondo, T. Seda, M. J. Chromatogr. 1985, 332, 107. Anderson, I. G. M. Supercritical fluid extraction coupled to packed column supercritical fluid chromatography. In Supercritical Fluid Extraction and Its Use in Chromatographic Sample Preparation Westwood, S. A. Ed., Blackie Academic and Professional, Chapman and Hall UK, 1993 p. 112. 

The separation and estimation of diloxanide furoate and metronidazole in solid dosage forms was reported by Bhoir et al., using packed column supercritical fluid chromatography [38], A JASCO Cig colunm (10 pm particle size, 25 cm x 4 mm) was used at 40°C, with an injection volume of 20 pL. The mobile phase consisted of 26% methanol in CO2 (flow rate of 2 mL/min), and operated at a pressure of 17.6 MPa. When detected on the basis of its ultraviolet absorbance at 230 nm, the retention time for the drug was 1.6 minutes. The linear region of the calibration graph was reported to be 20-70 pg/mL. 

MW Raynor, R Moulder, IL Davies, JP Kithinji, JE Hall, AA Clifford, KD Bartle. Dual capillary column supercritical fluid chromatography. Tenth symposium on capillary chromatography. Ed P Sandra, G Redant. Heidelberg Alfred Huethig Verlag, 1989, 1366-1382. 

R.M. Smith and M.M Sanagi, Application of packed column supercritical fluid chromatography to the analysis of barbituates, J. Pharm. Biomed. Anal., 6 837 (1988). 

T.A. Berge and J. F. Deye, Correlation between column surface area and retention of polar solutes in packed-column supercritical fluid chromatography, J. Chromatogr., 594 291 (1992). 

P. Biermanns, C. Miller, V. Lyon, and W. Wilson, Chiral resolution of /3-blockers by packed-column supercritical fluid chromatography, LC-GC Mag., 7/(10) 744 (1993). 

O. Gyllenhaal and J. Vessman, Packed-column supercritical fluid chromatography of omeprazole and related compounds selection of column support with triethylamine and methanol-modified carbon dioxide as the mobile phase, J. Chromatogr., 628 215 (1993). 

Biermanns et al. reported the chiral resolution of /3-blockers, including propranolol, metoprolol, and atenolol using packed-column supercritical fluid chromatography [38]. A Chiracel OD column with a mobile phase of 30% methanol with 0.5% isopropylamine in carbon dioxide was used for the separation. A baseline separation of isomers was obtained in less than 5 min at a mobile-phase flow rate of 2 ml/min. While keeping the column outlet pressure constant, the flow rate was increased to 4 ml/min and it was noted that, although the retention was reduced, the resolution remained the same. Both R- and S-propranolol gave linear responses from 0.25-2500 ppm with a correlation coefficient of >0.9999. The detection limit was approximately 250 ppb for a S/N ratio of 3. The reproducibility for both R- and S-propranolol was less than 1.5%. It was also noted that 0.09% R-propranolol can be quantitated in the presence of 2500 ppm of S-Propranolol. 

G.A. MacKay and G. D. Reed, Application of capillary supercritical fluid chromatography, packed column supercritical fluid chromatography, and capillary supercritical fluid chromatography-mass spectrometry in the analysis of controlled drugs, J. High Resolut. Chromatogr., 14 531 (1991). 

S. Scalia and D.E. Games, Determination of free bile acids in pharmaceutical preparation by packed column supercritical fluid chromatography, J. Pharm. Sci., 82 44 (1993). 

Xu X, Roman JM, Veenstra TD, Van Anda J, Ziegler RG, Issaq HJ (2006) Analysis of fifteen estrogen metabolites using packed column supercritical fluid chromatography-mass spectrometry. Anal Chem 78 1553-1558... 

Biermanns, E., Miller, C., Lyons, V., and Wilson, W.H. 1993. Chiral resolution of 3-blockers by packed column supercritical fluid chromatography. Liquid Chromatography Gas Chromatography, 10 744—7. 

Coombs, M.T., Khorassani, M.A., and Taylor, L.T. 1997. Packed column supercritical fluid chromatography-miass spectroscopy A review. Journal of Chromatography A, 785 85-100. 

Geiser, F.O., Yocklovich, S.G., Lurcott, S.M., Guthrie, J.W., Guthrie, E.J., and Levy, E.J. 1988. Water as a stationary phase modifier in packed-column supercritical fluid chromatography I. Separation of free fatty acids. Journal of Chromatography, 459 173-81. 

Oudsema, J. and Poole, C. 1992. Some practical experiences in the use of a solventless injection system for packed column supercritical fluid chromatography. Journal of High Resolution Chromatography, 15 65-70. 

Wheeler, J.R. and McNally, M.E. 1987. Comparison of packed column and capillary column supercritical fluid chromatography and high-performance hquid chromatography using representative herbicides and pesticides as typical moderate polarity and molecular weight range molecules. Journal of Chromatography, 410 343-53. 

J. Xu, R. Thompson, B. Li, and Z. Ge, Application of packed column supercritical fluid chromatography for separation of bromosulfone from process related impurities, /. Liq. Chrom. Relat. Technol. 25 (2002), 1007-1018. 

Carrott, M.J. Jones, D.C. Davidson, G. Identification and analysis of polymer additives using packed-column supercritical fluid chromatography with APCI mass spectro-metric detection. Analyst 1998, 123, 1827-1833. 

Fig. 1 Chromatogram of PAHs, herbicides, and phenols obtained by supercritical carbon dioxide modified with methanol. [Reprinted from L. Toribio, M. J. del Nozal, J. L. Bernal, J. J. Jimenez, and M. L. Serna, Packed-column supercritical fluid chromatography coupled with solid-phase extraction for the determination of organic microcontaminants in water,...

Several kinds of flavonoids are efficiently separated and analyzed using packed or capillary column supercritical fluid chromatography. The composition of mobile phase, stationary phase, temperature, and pressure aU affect the resolution. This article mainly focuses on the separation of polymethoxylated flavones, polyhydroxyl flavonoids, and flavonol isomers. 

---