Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications

Alan Rodrigo García-Cicourel; Bas van de Velde; Gerry Roskam; Hans Gerd Janssen

doi:10.1016/j.chroma.2019.460713

Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications

Alan Rodrigo García-Cicourel^*, Bas van de Velde, Gerry Roskam, Hans Gerd Janssen

^*Corresponding author for this work

Research output: Contribution to Journal › Article › Academic › peer-review

Abstract

Mineral oil hydrocarbons are used in the consumer goods sector for the elaboration of a wide range of foods and cosmetics. Traditional methods for determining their levels and composition are time consuming and laborious, besides requiring complex instrumentation. Here a simple and fast method was developed that uses columns packed with silver-modified silica in supercritical fluid chromatography with flame ionization and UV detection (SFC-FID/UV) for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in purified mineral oil samples. The method requires no sample preparation apart from dilution. Direct quantification of MOSH and MOAH was possible for samples with MOSH/MOAH ratios around one. For other samples deconvolution of the MOSH and MOAH humps in the FID chromatogram using the UV signal was needed since baseline separation of the two fractions could not be obtained. Validation of the method performance showed an excellent linearity (R² > 0.9995) in the range of concentrations tested (2.5–100 mgmL⁻¹) and a better repeatability than the standard methods (<5%). MOAH detection limits were better than 0.36% MOAH, which makes the method sufficiently sensitive for analysis of all but the highest purity mineral oils. The proposed SFC-FID/UV method was suitable for the analysis of mineral oils with viscosities and molecular weights below approximately 56 mm²s⁻¹ and 450 gmol⁻¹. The quantitative results of the new method were not statistically significantly different from those obtained with the standard SPE-GC-FID method where the new method has the advantages of a better repeatability, simpler operation and a significantly shortened analysis time. This new method could potentially also be used for the analysis of mineral oil contaminations in consumer products such as foods. However, in this case additional sample clean-up and preconcentration steps are needed for reducing matrix interferences from e.g. triglycerides and olefins and for improving the detection limits.

Original language	English
Article number	460713
Journal	Journal of Chromatography A
Volume	1614
DOIs	https://doi.org/10.1016/j.chroma.2019.460713
Publication status	Published - 15 Mar 2020
Externally published	Yes

Bibliographical note

Funding Information:
The authors thank the Consejo Nacional de Ciencia y Tecnolog?a de M?xico (CONACyT) for the scholarship awarded to A.R. Garc?a-Cicourel (No. 410740). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. This research did not receive any further specific grant from funding agencies in the public, commercial, or not-for-profit sectors.

Funding Information:
The authors thank the Consejo Nacional de Ciencia y Tecnología de México ( CONACyT ) for the scholarship awarded to A.R. García-Cicourel (No. 410740 ). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments.

Publisher Copyright:
© 2019

Funding

The authors thank the Consejo Nacional de Ciencia y Tecnolog?a de M?xico (CONACyT) for the scholarship awarded to A.R. Garc?a-Cicourel (No. 410740). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. This research did not receive any further specific grant from funding agencies in the public, commercial, or not-for-profit sectors. The authors thank the Consejo Nacional de Ciencia y Tecnología de México ( CONACyT ) for the scholarship awarded to A.R. García-Cicourel (No. 410740 ). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments.

Funders	Funder number
Consejo Nacional de Ciencia y Tecnología	410740
Consejo Nacional de Ciencia y Tecnología

Keywords

Argentation chromatography
Mineral oil analysis
MOSH/MOAH deconvolution
Parallel detection
Supercritical fluid chromatography

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10.1016/j.chroma.2019.460713

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García-Cicourel, A. R., van de Velde, B., Roskam, G., & Janssen, H. G. (2020). Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications. Journal of Chromatography A, 1614, Article 460713. https://doi.org/10.1016/j.chroma.2019.460713

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title = "Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications",

abstract = "Mineral oil hydrocarbons are used in the consumer goods sector for the elaboration of a wide range of foods and cosmetics. Traditional methods for determining their levels and composition are time consuming and laborious, besides requiring complex instrumentation. Here a simple and fast method was developed that uses columns packed with silver-modified silica in supercritical fluid chromatography with flame ionization and UV detection (SFC-FID/UV) for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in purified mineral oil samples. The method requires no sample preparation apart from dilution. Direct quantification of MOSH and MOAH was possible for samples with MOSH/MOAH ratios around one. For other samples deconvolution of the MOSH and MOAH humps in the FID chromatogram using the UV signal was needed since baseline separation of the two fractions could not be obtained. Validation of the method performance showed an excellent linearity (R2 > 0.9995) in the range of concentrations tested (2.5–100 mgmL−1) and a better repeatability than the standard methods (<5%). MOAH detection limits were better than 0.36% MOAH, which makes the method sufficiently sensitive for analysis of all but the highest purity mineral oils. The proposed SFC-FID/UV method was suitable for the analysis of mineral oils with viscosities and molecular weights below approximately 56 mm2s−1 and 450 gmol−1. The quantitative results of the new method were not statistically significantly different from those obtained with the standard SPE-GC-FID method where the new method has the advantages of a better repeatability, simpler operation and a significantly shortened analysis time. This new method could potentially also be used for the analysis of mineral oil contaminations in consumer products such as foods. However, in this case additional sample clean-up and preconcentration steps are needed for reducing matrix interferences from e.g. triglycerides and olefins and for improving the detection limits.",

keywords = "Argentation chromatography, Mineral oil analysis, MOSH/MOAH deconvolution, Parallel detection, Supercritical fluid chromatography",

author = "Garc{\'i}a-Cicourel, {Alan Rodrigo} and {van de Velde}, Bas and Gerry Roskam and Janssen, {Hans Gerd}",

note = "Funding Information: The authors thank the Consejo Nacional de Ciencia y Tecnolog?a de M?xico (CONACyT) for the scholarship awarded to A.R. Garc?a-Cicourel (No. 410740). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. This research did not receive any further specific grant from funding agencies in the public, commercial, or not-for-profit sectors. Funding Information: The authors thank the Consejo Nacional de Ciencia y Tecnolog{\'i}a de M{\'e}xico ( CONACyT ) for the scholarship awarded to A.R. Garc{\'i}a-Cicourel (No. 410740 ). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. Publisher Copyright: {\textcopyright} 2019",

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Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications. / García-Cicourel, Alan Rodrigo; van de Velde, Bas; Roskam, Gerry et al.
In: Journal of Chromatography A, Vol. 1614, 460713, 15.03.2020.

Research output: Contribution to Journal › Article › Academic › peer-review

TY - JOUR

T1 - Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications

AU - García-Cicourel, Alan Rodrigo

AU - van de Velde, Bas

AU - Roskam, Gerry

AU - Janssen, Hans Gerd

N1 - Funding Information: The authors thank the Consejo Nacional de Ciencia y Tecnolog?a de M?xico (CONACyT) for the scholarship awarded to A.R. Garc?a-Cicourel (No. 410740). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. This research did not receive any further specific grant from funding agencies in the public, commercial, or not-for-profit sectors. Funding Information: The authors thank the Consejo Nacional de Ciencia y Tecnología de México ( CONACyT ) for the scholarship awarded to A.R. García-Cicourel (No. 410740 ). The authors acknowledge Joshka Verduin for her assistance with the SPE-GC-FID experiments. Publisher Copyright: © 2019

PY - 2020/3/15

Y1 - 2020/3/15

N2 - Mineral oil hydrocarbons are used in the consumer goods sector for the elaboration of a wide range of foods and cosmetics. Traditional methods for determining their levels and composition are time consuming and laborious, besides requiring complex instrumentation. Here a simple and fast method was developed that uses columns packed with silver-modified silica in supercritical fluid chromatography with flame ionization and UV detection (SFC-FID/UV) for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in purified mineral oil samples. The method requires no sample preparation apart from dilution. Direct quantification of MOSH and MOAH was possible for samples with MOSH/MOAH ratios around one. For other samples deconvolution of the MOSH and MOAH humps in the FID chromatogram using the UV signal was needed since baseline separation of the two fractions could not be obtained. Validation of the method performance showed an excellent linearity (R2 > 0.9995) in the range of concentrations tested (2.5–100 mgmL−1) and a better repeatability than the standard methods (<5%). MOAH detection limits were better than 0.36% MOAH, which makes the method sufficiently sensitive for analysis of all but the highest purity mineral oils. The proposed SFC-FID/UV method was suitable for the analysis of mineral oils with viscosities and molecular weights below approximately 56 mm2s−1 and 450 gmol−1. The quantitative results of the new method were not statistically significantly different from those obtained with the standard SPE-GC-FID method where the new method has the advantages of a better repeatability, simpler operation and a significantly shortened analysis time. This new method could potentially also be used for the analysis of mineral oil contaminations in consumer products such as foods. However, in this case additional sample clean-up and preconcentration steps are needed for reducing matrix interferences from e.g. triglycerides and olefins and for improving the detection limits.

AB - Mineral oil hydrocarbons are used in the consumer goods sector for the elaboration of a wide range of foods and cosmetics. Traditional methods for determining their levels and composition are time consuming and laborious, besides requiring complex instrumentation. Here a simple and fast method was developed that uses columns packed with silver-modified silica in supercritical fluid chromatography with flame ionization and UV detection (SFC-FID/UV) for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in purified mineral oil samples. The method requires no sample preparation apart from dilution. Direct quantification of MOSH and MOAH was possible for samples with MOSH/MOAH ratios around one. For other samples deconvolution of the MOSH and MOAH humps in the FID chromatogram using the UV signal was needed since baseline separation of the two fractions could not be obtained. Validation of the method performance showed an excellent linearity (R2 > 0.9995) in the range of concentrations tested (2.5–100 mgmL−1) and a better repeatability than the standard methods (<5%). MOAH detection limits were better than 0.36% MOAH, which makes the method sufficiently sensitive for analysis of all but the highest purity mineral oils. The proposed SFC-FID/UV method was suitable for the analysis of mineral oils with viscosities and molecular weights below approximately 56 mm2s−1 and 450 gmol−1. The quantitative results of the new method were not statistically significantly different from those obtained with the standard SPE-GC-FID method where the new method has the advantages of a better repeatability, simpler operation and a significantly shortened analysis time. This new method could potentially also be used for the analysis of mineral oil contaminations in consumer products such as foods. However, in this case additional sample clean-up and preconcentration steps are needed for reducing matrix interferences from e.g. triglycerides and olefins and for improving the detection limits.

KW - Argentation chromatography

KW - Mineral oil analysis

KW - MOSH/MOAH deconvolution

KW - Parallel detection

KW - Supercritical fluid chromatography

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ER -

Supercritical fluid chromatography as a rapid single-step method for the determination of mineral oil saturated and aromatic hydrocarbons in purified mineral oils for food and cosmetics applications

Abstract

Bibliographical note

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Keywords

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