Preparative chromatography packing columns

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). 

Time, Cost, and Equipment Analysis time can vary from several minutes for samples containing only a few constituents to more than an hour for more complex samples. Preliminary sample preparation may substantially increase the analysis time. Instrumentation for gas chromatography ranges in price from inexpensive (a few thousand dollars) to expensive (more than 50,000). The more expensive models are equipped for capillary columns and include a variety of injection options and more sophisticated detectors, such as a mass spectrometer. Packed columns typically cost 50- 200, and the cost of a capillary column is typically 200- 1000. 

Glass chromatography column 400 x 15-mm i.d. with a stopcock Column preparation A silica gel column is prepared by packing a slurry of silica gel (10 g) in n-hexane-acetone (9 1, v/v) into a glass chromatography column. About a 1-cm layer of anhydrous sodium sulfate is placed above and below the... 

Preparative chromatography is a powerful tool to isolate working quantities of compounds from complex samples. Preparative GC, which is normally carried out on packed columns, is useful for components with a b.p. < 450 °C and levels > 100 ppm (impossible for < lOppm questionable for 10-100ppm). Total amount needed is 2 p,L. 

The urine of people who are heavy smokers contains mutagenic chemicals, chemicals that cause mutations in biological cells. Bioanalytical laboratories can analyze urine samples for these chemicals, but the samples must be cleaned up first prior to extraction with methylene chloride. The procedure for this cleanup utilizes an open column chromatography. Columns several inches tall and about an inch wide are prepared by packing them with an adsorbing resin that has been treated with methyl alcohol. The urine samples are passed through these columns as part of the sample preparation scheme. 

A second field of rapid development in the l.c. of carbohydrates is in practical, preparative chromatography. Early preparative systems used large, expensive columns with low resolving power, and hence, were not extensively applied in carbohydrate research. New research is showing that various carbohydrates can be separated on the gram scale, using normal l.c. equipment and large columns home-packed with relatively... 

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. 

Larger diameter columns were also available for preparative chromatography. In later years, GPC analysis times were reduced and resolution was Improved by using shorter columns that were packed with smaller particle size material. A typical family of GPC columns that is available today contains 7pm particles... 

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