High pressure chromatography instrumentation

Supercritical fluid chromatography are more complex that HPLCs. One of the fluids is usually a liquefied gas at high pressure. The instrument cannot use a single high pressure pump and a gradient valve to mix such fluids with normal liquids. Consequently, one always requires at least two high pressure... 

The basic instrument required for packed-column unified chromatography is shown schematically in Figure 7.9. This is essentially a two-pump HPLC instrument utilizing high-pressure mixing with just a few new components. At least one pump must... 

Novolac molecular weights were measured in THF at 35°C by high pressure size exclusion chromatography using a Waters Model 510 pump (flow rate=1.0 ml/min), 401 differential viscometer detector and a set of Dupont PSM 60 silanized columns. A universal calibration curve was obtained with a kit of 10 narrow molecular weight distribution, linear polystyrene standards from Toya Soda Company. Data acquisition and analysis were performed on an AT T 6312 computer using ASYST Unical 3.02 software supplied with the Viscotek instrument. 

This chapter presents an overview of current trends in high-pressure liquid chromatography (HPLC) instrumentation focusing on recent advances and features relevant to pharmaceutical analysis. Operating principles of HPLC modules (pump, detectors, autosampler) are discussed with future trends. 

This chapter deals with the properties of high-pressure liquid chromatography columns. It is divided into two sections column physics and column chemistry. In the section on column physics, we discuss the properties that influence column performance, such as particle size, column length and column diameter, together with the effect of instrumentation on the quality of a separation. In the section on column chemistry, we examine in depth the surfaces of modern packings, as well as the newer developments such as zirconia-hased packings, hybrid packings or monoliths. We have also included a short section on... 

FSIS laboratories also use chemical techniques and instrumentation to identify select antibiotic residues. The tetracyclines of interest are identified by thin layer chromatography. Sulfonamides are detected and quantified by fluorescence thin lay chromatography and confirmed by gas chromatography/mass spectrometry. Amoxicillin and gentamycin are identified and/or quantified by high pressure liquid chromatography. Similar techniques are used to identify ionophores and other antimicrobials of interest. 

The application of atomic spectroscopic instruments as element-specific detectors in chromatography has been reviewed by van Loon More recently, Krull has extensively reviewed their use in high pressure liquid chromatography (HPLC). Atomic spectrometry has found wide acceptance in the field of liquid chromatography because, in most cases, the fractions can be directly analysed after elution from the column. However, it is possible to use the technique for the analysis of solid samples without first dissolving the matrix. This is particularly useful after electrophoresis, where the fractions are fixed either in a gel or on paper. Kamel et al. have shown that it is possible to cut the appropriate sections and insert them into the carbon furnace for analysis. The disadvantage of this approach is that the precision is usually poorer (about 10%) and it is difficult to calibrate the instrument. Nevertheless, this approach is very useful if it is used for qualitative speciation. 

The analysis of individual chemical constituents in distilled spirits currendy is performed using gas chromatography (gc) and high pressure liquid chromatography (hplc). Although other types of instrumental analyses have yielded much information regarding the chemical constituency of distilled spirits, the combination ofgc and hplc has allowed hundreds of different chemical components of distilled spirits to be individually identified and accurately quantified. 

It is for these reasons that a recommendation is made to avoid, wherever possible, concentration and cleanup steps that involve "column chromatography" of this nature, that is, chromatography where an in-line detector is not involved. This distinction is made to eliminate any implied criticism of instrumented high pressure liquid chromatographic systems which have not to date been used extensively for this particular purpose. 

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