Evaluation of a microHPLC system dedictaed to packed capillary column liquid chromatography

Trisciani, Adriano; Andreolini, Franca

doi:10.1002/jhrc.1240130412

Cited by 10 publications

(4 citation statements)

References 11 publications

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“…achieved under these conditions. The pressure and flow profiles throughout the analytical run were monitored for excessive excursions, the variations seen are considered to be acceptable for a reciprocating pump and are comparable to previously reported data [2,3]. The coefficient of variation of the retention time of the early eluting peaks is high; this is considered to be due to small errors in timing associated with the manual starting of the integrator after sample injection causing a large coefficient of variation for peaks with a short retention time.…”

Section: Resultssupporting

confidence: 79%

“…A number of approaches have been made to achieve this, principally divided into the use of micro pumps and of flow splitting techniques. A reciprocating micro pump has been described [3] which has a flow range of 1 pl to 4 mL; this gave very reproducible retention times, with a coefficient of variation of less than 1%. A similar type of system was described by Levy 141, but this had the limitation of a minimum flow of 10 pl/min.…”

Section: Introductionmentioning

confidence: 99%

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Modifier addition in microcolumn supercritical fluid chromatography

Robson¹,

Raynor²,

Bartle³

et al. 1995

J Microcolumn Separations

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Abstract. Recent advances in techniques for the packing of microcolumns of down to 50 p m inner diameter using supercritical CO, have led to rapid growth in the use of high efficiency packed capillary columns in SFC. Maximization of the usefulness and applications of these techniques requires gradient elution chromatography and the development of pumps capable of delivering 0.1 to 1 pl per minute of modifier. A micro SFC-LC pump has been tested in the isocratic and gradient elution mode with CO, as the supercritical fluid and methanol as the modifier. The pump was tested using the EPA priority PAHs as the test mixture with a specially treated ODS column and UV detection. Results are presented for testing in the isocratic and gradient elution modes and the retention times are shown to have a coefficient of variation of less than 2%. The application of this system to the analysis of PAHs in coal derivatives is shown. The problems encountered in the use of formic acid as a modifier in SFC are discussed. c) 109.5

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Section: Resultssupporting

confidence: 79%

Section: Introductionmentioning

confidence: 99%

Modifier addition in microcolumn supercritical fluid chromatography

Robson¹,

Raynor²,

Bartle³

et al. 1995

J Microcolumn Separations

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“…For the example, Yang et al [136] and Verzele et al [137] applied the microbore column packing miniaturation for the MD sampling analysis; Novotny M et al [138] and Krejci et al [139] applied the microcolumns in liquid chromatography analysis. Trisciani et al [140] applied the micro-HPLC system to packed capillary column liquid chromatography to study the solvents delivery systems. Chaurasia et al [141] used the MD-HPLC-ECD to monitor the conscious and freely moving rats the in vivo monoamine neurotransmitters and its metabolites contents changes.…”

Section: The Microdialysis Technique Coupled With the Newlymodernizedmentioning

confidence: 99%

Crosstalk the Microdialysis in Scientific Research: from Principle to its Applications

Lee¹,

Di²

2013

Pharm Anal Acta

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“…Numerous packed capillary HPLC/MS systems and applications have been described previously. [12][13][14][15][16][17][18][19][20][21][22] However, most have required complex specialized solvent delivery systems and tedious chromatographic system construction procedures to realize the advantages of reduced solvent consumption and dramatic enhancement of chromatographic performance over conventional analytical scale techniques. Due to this complexity, previous approaches require dedication of both operator and instrument if routine use is to be realized, a situation ill afforded by the resource-constrained multi-disciplinary MS laboratory.…”

mentioning

confidence: 99%

Design, construction and application of a simple packed capillary high performance liquid chromatography/electrospray mass spectrometry system

Robins¹,

Guido²

1997

Rapid Commun. Mass Spectrom.

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A simple packed-capillary high performance liquid chromatography (HPLC) system for the analysis of trace (picogram) mixtures by electrospray mass spectrometry is described in detail. This simple and cost-effective design is constructed from conventional hardware generally available in the modern LC/MS laboratory. Short slurry-packed vitreous silica capillary columns (5 cm ؋ 200 µm i.d.) are prepared in minutes from a variety of commercial bulk packing materials by fast, medium pressure bomb packing. Precise submicroliter per minute gradient elution of the capillary column is achieved by precolumn flow splitting of a conventional, analytical-scale, gradient HPLC pump operating at 0.5 to 3.0 mL/min. flow rates. Chromatographic system dead volume is reduced to a minimum via unique integration of the splitter, injector, capillary column and electrospray emitter into a single assembly, thereby markedly improving chromatographic performance and ease of use. System performance is demonstrated through several applications, including the determination of caffeine in untreated urine, the analysis of tryptic peptide mixtures harvested from electrophoretic gels and the determination of trace impurities in pharmaceutical bulk drugs. © 1997 by John Wiley & Sons, Ltd. This laboratory provides structural characterization support for the research and development of a wide range of pharmaceutical agents including both conventional 'small molecule' synthetics and biopolymers derived from recombinant technology. As such, we are routinely challenged by the demand for rapid and cost effective analyses of complex mixtures spanning diverse chemical classification. Such analyte diversity has required the implementation of nearly all sample ionization and 'hyphenated' introduction methods, the number of which precludes the luxury of maintaining costly, functionally dedicated mass spectrometry (MS) systems.This challenge has intensified due to acceleration of the pharmaceutical development process, prolific drug template expansion through combinatorial chemistry, and the need for decisive metabolite and degradant characterization in early high volume testing models and preclinical formulation design studies. Such early investigations are further hindered by severe sample size limitations rendered tractable only through marked chromatographic scale reduction.While several 'nano-scale' liquid separation methods have been successfully interfaced with mass spectrometry for such purposes including capillary electrophoresis (CE), supercritical fluid chromatography (SFC), and capillary electrochromatography (CEC), packed capillary HPLC methods with electrospray ionization (ESI) mass spectrometric detection are the most versatile and easiest to implement.1-11 HPLC and ESI-MS are well suited to each other and to the analysis of the widest range of highly functionalized, thermally labile, and reactive biologically active species. Adsorption mode HPLC, arguably the dominant modern chromatographic separation method, has the further advantage of being ...

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Evaluation of a microHPLC system dedictaed to packed capillary column liquid chromatography

Cited by 10 publications

References 11 publications

Modifier addition in microcolumn supercritical fluid chromatography

Modifier addition in microcolumn supercritical fluid chromatography

Crosstalk the Microdialysis in Scientific Research: from Principle to its Applications

Design, construction and application of a simple packed capillary high performance liquid chromatography/electrospray mass spectrometry system

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