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31. Use of porous graphitic carbon coupled with mass detection for the analysis of polar phenolic compounds by liquid chromatography

Author

Amadeo R. Fernández-Alba, Marie-Claire Hennion, Ana Agüera, and Jérôme Vial

Subjects
Chemical ionization, Chromatography, Organic Chemistry, Analytical chemistry, Reproducibility of Results, Atmospheric-pressure chemical ionization, General Medicine, Phenolic acid, Mass spectrometry, Biochemistry, High-performance liquid chromatography, Mass Spectrometry, Analytical Chemistry, Matrix (chemical analysis), chemistry.chemical_compound, Phenols, chemistry, Graphite, Tetrahydrofuran, Chromatography, Liquid
Abstract

Phenolic compounds present in olive mill wastewater (OMW) need to be quantified because of their pollution capacity toward the environment. In the present study, six representative phenolic compounds of OMW were chosen to develop a LC-MS method. The high polarity of the compounds caused problems when using traditional reversed-phase liquid chromatography (RPLC). Consequently, a method was developed on another kind of chromatographic phase: Porous Graphitic Carbon (PGC) involving the use of a tetrahydrofuran (THF) gradient. The influence of THF as mobile phase in LC-MS coupling, which is not common practice, was evaluated. In Atmosperic Pressure Chemical Ionisation (APCI) in the negative ion mode, the presence of THF in the mobile phase did not degrade the MS signal of the target compounds in the conditions studied. On the contrary, an improvement was even observed when the percentage of THF increased. The proposed PGC-LC-MS method was selective and linear for the six phenolic compounds analysed with limits of quantification lower than 5 ppm in all cases. The precision was satisfactory (pooled RSD around 6%). The analyses of OMW matrix spiked sample confirmed the good performance of the proposed method.

Published
2001
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32. Methodology for transfer of liquid chromatography methods based on statistical considerations

Author

Andre Brun, A. Jardy, Jean-Michel Menet, Jérôme Vial, and Pascal Anger

Subjects
Chromatography, Chemistry, Organic Chemistry, General Medicine, Certification, Biochemistry, Analytical Chemistry, Task (project management), Quantitative analysis (finance), Long period, Transfer (computing), Compatibility (mechanics), Statistical dispersion, Statistic
Abstract

An important task in the pharmaceutical industry today is analytical transfer. However, no actual guidelines are available today. It is for this reason that we decided to devise a rigorous method using statistic exploitation of results. The statistical technique used is ANOVA (analysis of variance). We chose to treat the case of quantitative analysis in LC but the methodology could easily be adapted to other analytical techniques. The criteria of the transfer validation could be formulated thus: “for each response of interest, the new laboratory must produce results that are not significantly different from those of the reference entity”, or more explicitly by: “the new laboratory must have dispersion characteristics compatible with those of the reference entity and must exhibit no bias”. While compatibility of precision can easily be assessed, the test of absence of bias requires that certified materials be available. Since certified materials can only be obtained through an inter-laboratory study, it means that the reference entity is necessarily a pool of laboratories. Using a single laboratory instead of a pool would not allow a distinction to be drawn between a bias and an inter-laboratory dispersion, which would lead to abnormal transfer failure. The methodology developed was then used on an example. The last part deals with the situation where certified materials are suspected to be slightly degraded. It is explained how such a case, likely to be encountered in pharmaceutical products stored over a long period, can be handled without re-starting the study from scratch.

Published
1998
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