Rapid separations of respectable efficiency for nonvolatile solutes can be achieved by use of capillary columns in conjunction with supercritical fluids Capillary columns were first described for gas chromatography (GC) in 1957 by M.J.E. Golay, who utilized long, open tubular columns uniformly coated with a thin layer of stationary phase (1). Although many technological improvements were necessary in the years following Golay's invention, the method has recently revolutionized many areas of scientific research. This is primarily due to its high resolving power, allowing the separation, detection, and quantitation of hundreds of components from a sample in a single chromatogram.
The bask Instrument components requlred for caplllary supercrltlcal fluld chromatography include a high-pressure pump with pressure programmer, a small-volume sample Inlet system, a constant temperature oven, and a small-volume detector. The major stresses applied to the hstrumentatlon are the hlgh pressures and temperatures required to maintain the mobile phase at or above Its crltlcal polnt. Of the dlfferent sample introductlon systems studied, spllt Injection presently appears to be the most effectlve. By use of the described hstrumentatlon, a plate helght of 0.30 mm was obtalned for pyrene ( k = 0.50) on a 100-hm caplllary column contalnlng a bonded poly(methylphenylslloxane) statlonary phase.
A newly developed portable capillary liquid chromatograph was investigated for the separation of various pharmaceutical and illicit drug compounds. The system consists of two high‐pressure syringe pumps capable of delivering capillary‐scale flow rates at pressures up to 10 000 psi. Capillary liquid chromatography columns packed with sub‐2 μm particles are housed in cartridges that can be inserted into the system and easily connected through high‐pressure fluidic contact points by simply applying a specific, predetermined torque rather than using standard fittings and less precise sealing protocols. Several over‐the‐counter analgesic drug separations are demonstrated, along with a simple online measurement of tablet dissolution. Twenty illicit drug compounds were also separated across six targeted drug panels. The results described in this study demonstrate the capability of this compact liquid chromatography instrument to address several important drug‐related applications while simplifying system operation, and greatly reducing solvent usage and waste generation essential for onsite analysis.
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