Microliter sample introduction for open tubular column supercritical fluid chromatography using a packed capillary for solute focusing (original) (raw)
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Instrumental aspects of capillary supercritical fluid chromatography
Analytical Chemistry, 1982
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.
Supercritical fluid chromatography in pharmaceutical analysis
Journal of pharmaceutical and biomedical analysis, 2015
In the last few years, there has been a resurgence of supercritical fluid chromatography (SFC), which has been stimulated by the introduction of a new generation of instruments and columns from the main providers of chromatographic instrumentation, that are strongly committed to advancing the technology. The known limitations of SFC, such as weak UV sensitivity, limited reliability and poor quantitative performance have been mostly tackled with these advanced instruments. In addition, due to the obvious benefits of SFC in terms of kinetic performance and its complementarity to LC, advanced packed-column SFC represents today an additional strategy in the toolbox of the analytical scientist, which may be particularly interesting in pharmaceutical analysis. In the present review, the instrumentation and experimental conditions (i.e. stationary phase chemistry and dimensions, mobile phase nature, pressure and temperature) to perform "advanced SFC" are discussed. The applicabil...
Analytical Science Advances
The first discussions on the use of inorganic gases above their critical point as mobile phase in chromatography systems stems back to 1957 1 and it was Klesper et al who reported on a preliminary study in which chlorofluorocarbons were used above their critical point to separate metal phophorins. 2 Supercritical fluid chromatography (SFC) with carbon dioxide as the mobile phase emerged in the late 1960s. In the past decade, a new generation of SFC instruments are commercially available and also the number of applications of SFC have grown considerably. Here, Susan Olesik, Caroline West, Davy Guillarme, Debby Mangelings, and Lucie Nováková share their thoughts on the technology and discuss the challenges and potential of SFC. 1 WHAT WAS YOUR FIRST EXPERIENCE WITH SFC? Susan Olesik: I joined Milos Novotny's group in 1982. This was in the very early days of capillary Supercritical fluid chromatography. While I was in the Novotny group, we published the first SFC-FTIR interface. Caroline West: I started doing SFC as a PhD student. It was the only technique I was supposed to investigate for my thesis. I was drawn to the topic because my mentor convinced me that it was a technique worth learning, because there were still lots of unknowns. As one who This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.
Supercritical fluid chromatography in drug analysis: a literature survey
Analytical and Bioanalytical Chemistry, 1996
The applications of supercritical fluid chromatography to the analysis of drugs have been carefully revised from the literature compiled in the Analytical Abstracts until March 1994. Easy-to-read tables provide useful information about the state-of-the-art and possibilities offered by SFC in pharmaceutical analysis. The tables comprise extensive data about samples analyzed, pharmaceutical principles determined, solvents used and sample quantity injected, supercritical fluids and modifiers employed, injection system, instrumentation, experimental conditions for chromatographic separations (density, pressure, flow, temperature), characteristics of columns employed (type, support, length, diameter, particle film thickness, stationary phase), detectors, type of restrictors, and also some analytical features of the methods developed (such as retention time, resolution, sensitivity, limit of detection and relative standard deviation).
The many faces of packed column supercritical fluid chromatography - A critical review
Journal of chromatography. A, 2015
Packed column sub- and supercritical fluid chromatography (SFC) is a versatile separation method: on the one hand the number of parameters acting on the quality of a separation is very large, and the effects of these parameters can be complex (and not always fully understood). But on another hand, due to numerous advantageous properties of CO2-based mobile phases, method development is a fast task. This paper is a review of the main features of SFC, focusing essentially on achiral separations. However, several fundamental aspects discussed here are also relevant to chiral SFC separations. This is not intended to be an extensive review, as the way to practice SFC has somewhat evolved with time. We rather wished to provide an expert opinion on the characteristics of the method, pointing at the sources of difficulty and displaying the wide possibilities that it offers. A large number of selected applications concerning several different areas are also presented.
History of supercritical fluid chromatography: Instrumental development
In the early days of supercritical fluid chromatography (SFC), it was categorized as high-pressure or dense gas chromatography (HPGC or DGC) and low boiling point hydrocarbons were used as supercritical mobile phase. Various liquids and gases were examined, however, by the late 1970s, carbon dioxide (CO2) became the most preferred fluid because it has low critical temperature (31.1C) and relatively low critical pressure (7.38 MPa); in addition, it is non-toxic, nonflammable and inexpensive. A prototype of a modern packed-column SFC instrument appeared in the late 1970s. However, in the 1980s, as open tubular capillary columns appeared and there was keen competition with packed columns. And packed-column SFC at once became less popular, but it regained popularity in the early 1990s. The history of SFC was of “the rise and fall.” Advances in chiral stationary phase took place in the early 1990s made packed-column SFC truly useful chiral separation method and SFC is now regarded as an inevitable separation tool both in analytical and preparative separation.