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Original Articles

A New Small Coil‐Volume CCC Instrument for Direct Interfacing with MS

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Pages 1345-1354 | Received 29 Jun 2002, Accepted 02 Oct 2002, Published online: 06 Feb 2007
 

Abstract

One of the major factors restricting the use of CCC as an analytical tool is the speed at which a separation may be conducted. This paper describes the phased development of a new low volume capacity Milli‐CCC device, which is as rapid as HPLC, achieving high resolutions in minutes as opposed to hours, with the capability of linking with a mass spectrometer (CCC/MS). The Milli‐CCC J‐type apparatus has gears enclosed in a lubricated case to minimize noise. Its volume with one coil mounted in a cantilever style is 4.6 mL with 2.5 m of 0.76 mm bore tubing. It can rotate at a maximum speed of 2100 rpm. Stationary phase retention factor higher than 60% could be obtained with 1500 rpm and 1 mL/min producing separation of compounds with K D distribution coefficient of 1 in less than 5 min. The connection to MS was straightforward.

Acknowledgments

This research, and the development of the Milli‐CCC, was carried out with grant support from the EPSRC Grant No. GR/M48345 ID13, entitled “A New Rapid Centrifugal Liquid–Liquid Chromatography Separation and Detection System for Multiple High Resolution Purification Without Sample Loss or Degradation.” The authors are grateful to the EU INTAS programme No. 00‐0782 entitled “Fundamental Research into the Hydrodynamics and Efficiency of Counter‐Current Chromatography” for supporting the working visit of Dr. Svetlana Ignatova who carried out the stationary phase retention and resolution studies.

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