General Concepts in Column Chromatography

Poole, Colin F.

doi:10.1016/b978-044450198-1/50014-8

Cited by 11 publications

(5 citation statements)

References 250 publications

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“…Hence, we conclude that the sample introduction system is responsible for the observed tailing in the ion chromatograms and it is not caused by the analyte separation on the column. The tailing in the introduction system leads to a decrease in chromatographic resolution 34 (calculated from the peak width at half height) from e.g. 3.3 between the FA and AA peaks in the UV chromatogram to 0.8 in the MS signals.…”

Section: Resultsmentioning

confidence: 99%

Implementation of an enclosed ionization interface for the analysis of liquid sample streams with direct analysis in real time mass spectrometry

Kloth

Khanipour

Mayrhofer

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale:The development of an interface to introduce liquid sample streams to direct analysis in real time mass spectrometry (DART-MS) is of great interest for coupling various analytical techniques, using non-volatile salts, with MS. Therefore, we devised an enclosed ionization interface and a sample introduction system for the versatile analysis of liquid samples with DART-MS. Methods: The sample introduction system consists of a nebulizer, a spray chamber and a transfer line, while the confined ionization interface is created by implementing a cross-shaped housing between the ion source and the MS inlet. Methodical studies of the effects of various setup parameters on signal intensity and peak shape were conducted, while its diverse applicability was demonstrated by coupling with high-performance liquid chromatography (HPLC) for the analysis of alcohols, organic acids and furanic compounds. Results: The confinement of the ionization interface results in a robust setup design with a well-defined ionization region for focusing of the sprayed sample mist. Thereby, an increase in analyte signal intensity by three orders of magnitude and improved signal stability and reproducibility were obtained in comparison to a similar open ionization interface configuration. Additionally, the successful quantification of alcohols could be demonstrated as well as the compatibility of the setup with HPLC gradient elution. Conclusions: A versatile setup design for the analysis of liquid sample streams with DART-MS was devised for monitoring reactions or hyphenating analytics with MS. It minimizes This article is protected by copyright. All rights reserved.interferences from the laboratory surrounding as well as allows for safe handling of hazardous and toxic chemicals, which renders it suitable for a broad range of applications.

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Section: Resultsmentioning

confidence: 99%

Implementation of an enclosed ionization interface for the analysis of liquid sample streams with direct analysis in real time mass spectrometry

Kloth

Khanipour

Mayrhofer

et al. 2021

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

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“…These parameters were included in the chromatographic response function (CRF) for evaluation of the performance of our method (Poole, 2003). These parameters were included in the chromatographic response function (CRF) for evaluation of the performance of our method (Poole, 2003).…”

Section: Methods Developmentmentioning

confidence: 99%

“…In this case, the equation had the following distribution: Parameters in the model were final chromatographic time, resolution between each peak and the number of peaks. These parameters were included in the chromatographic response function (CRF) for evaluation of the performance of our method (Poole, 2003).…”

Section: Methods Developmentmentioning

confidence: 99%

“…Three model intervals were used for the evaluation of recovery at low, medium and high concentrations (Poole, 2003). Three model intervals were used for the evaluation of recovery at low, medium and high concentrations (Poole, 2003).…”

Section: Accuracymentioning

confidence: 99%

“…Accuracy was evaluated by calculation of the recovery factors determined by spiking placebo samples with the concentrations that showed linearity. Three model intervals were used for the evaluation of recovery at low, medium and high concentrations (Poole, 2003).…”

Section: Accuracymentioning

confidence: 99%

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New approach for determination of the degradation products of fenspiride hydrochloride found in oral liquid formulations

Cioroiu

Caba

Prisăcaru

et al. 2018

Biomedical Chromatography

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Fenspiride hydrochloride (FNS) is used in treating chronic inflammatory diseases, most commonly as a liquid oral solution. FNS produces degradation products along with fenspiride N-oxide (FNO) and 1-phenylethyl-4-hydroxy-4-aminomethyl piperidine hydrochloride (PHAP). We aimed to develop and validate a chromatographic method in order to identify the main degradation products in the presence of other compounds from a liquid preparation. The method used a dual gradient using two buffer solutions: the first with pH 4.5 (buffer 1, pH 4.5-MeOH 90:10%, v/v) and the second with pH 2.9 (buffer 2, pH 2.9-acetronitrile-methanol, 65:15:10%, v/v/v). As mentioned, there was a modification of the organic mixture, starting with 10% methanol and ending with a mixture of acetonitrile-methanol (15:10%, v/v). The flow-rate was 1.5 mL/min. According to the elution program, experimental conditions started with 100% solution S1, which decreased to 0% and, simultaneously, solution S2 increased to 100% during the first 10 min and was maintained for a further 5 min. After 15 min, initial conditions were re-established. The linearity interval was 0.5-2 μg/mL and the minimum correlation coefficient was 0.999. The recovery factor was 100.47-103.17% and the limit of quantification was 0.19-0.332 μg/mL. Intra-day maximum precision was 4.08% for FNS and 2.65% for PHAP. This double-gradient mobile phase produced good specificity in relation to the degradation products of FNS and other constituents of the oral liquid formulation. Forced degradation studies revealed other related substances that were confirmed in mass balance analyses. Degradation products were confirmed in acidic, basic and oxidative media.

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Factors Influencing the Isothermal Retention Indices of 51 Solutes on 12 Stationary Phases of Different Polarity: Applicability of the Solvation Parameter Model

et al. 2015

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General Concepts in Column Chromatography

Cited by 11 publications

References 250 publications

Implementation of an enclosed ionization interface for the analysis of liquid sample streams with direct analysis in real time mass spectrometry

Implementation of an enclosed ionization interface for the analysis of liquid sample streams with direct analysis in real time mass spectrometry

New approach for determination of the degradation products of fenspiride hydrochloride found in oral liquid formulations

Factors Influencing the Isothermal Retention Indices of 51 Solutes on 12 Stationary Phases of Different Polarity: Applicability of the Solvation Parameter Model

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