Use of a guard column coupled to mass spectrometry as a fast semi-quantitative methodology for the determination of plasticizer metabolites in urine
Copyright © 2023 The Author(s). Published by Elsevier B.V. All rights reserved..
For the first time, a very simple and fast method combining the use of a guard column coupled to tandem mass spectrometry (guard column-MS/MS) has been proposed for the determination of plasticizer metabolites in urine. Briefly, samples (1.0 mL) were submitted to enzymatic hydrolysis for 10 min, filtered, diluted 1/10 v/v with ultrapure water and directly injected into the system. A fast run of only 2 min (3 min including the injection cycle) allowed the determination of 19 analytes. Enzymatic hydrolysis, filtering material, and guard column-MS/MS conditions were optimized. Intra-day precision at the low-level concentration (expressed as relative standard deviation, %RSD) obtained from the analysis of synthetic urine samples varied between 11 and 20%. Limits of quantification ranged from 2.8 to 60 ng/mL. Trueness values, calculated as apparent recoveries, ranged from 70 to 135%. To correct for matrix effects, analyte concentrations in real urine were quantified by the standard addition method. To confirm the results obtained by guard column-MS/MS, an ultra(high)-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was also applied (total chromatographic run time 17 min, including column re-equilibration). Concentrations measured with both methods were in good agreement. Hence, we propose the use of guard column-MS/MS to analyse a large number samples in a very short time (semi-quantification), and apply the chromatographic analysis only to those samples with levels close to/higher than the concentrations equivalent to the safe maximum daily intakes of the parent compounds (confirmation). This double strategy (semi-quantification by guard column-MS/MS and confirmation-when needed-by UHPLC-MS/MS) implies important savings in time and money.
| Medienart: |
E-Artikel |
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| Erscheinungsjahr: |
2023 |
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| Erschienen: |
2023 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:1690 |
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| Enthalten in: |
Journal of chromatography. A - 1690(2023) vom: 08. Feb., Seite 463788 |
| Sprache: |
Englisch |
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| Beteiligte Personen: |
González-Mariño, Iria [VerfasserIn] |
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| Links: |
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| Themen: |
Guard column |
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| Anmerkungen: |
Date Completed 03.02.2023 Date Revised 03.02.2023 published: Print-Electronic Citation Status MEDLINE |
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| doi: |
10.1016/j.chroma.2023.463788 |
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| funding: |
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| Förderinstitution / Projekttitel: |
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NLM351604820 |
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| 520 | |a Copyright © 2023 The Author(s). Published by Elsevier B.V. All rights reserved. | ||
| 520 | |a For the first time, a very simple and fast method combining the use of a guard column coupled to tandem mass spectrometry (guard column-MS/MS) has been proposed for the determination of plasticizer metabolites in urine. Briefly, samples (1.0 mL) were submitted to enzymatic hydrolysis for 10 min, filtered, diluted 1/10 v/v with ultrapure water and directly injected into the system. A fast run of only 2 min (3 min including the injection cycle) allowed the determination of 19 analytes. Enzymatic hydrolysis, filtering material, and guard column-MS/MS conditions were optimized. Intra-day precision at the low-level concentration (expressed as relative standard deviation, %RSD) obtained from the analysis of synthetic urine samples varied between 11 and 20%. Limits of quantification ranged from 2.8 to 60 ng/mL. Trueness values, calculated as apparent recoveries, ranged from 70 to 135%. To correct for matrix effects, analyte concentrations in real urine were quantified by the standard addition method. To confirm the results obtained by guard column-MS/MS, an ultra(high)-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was also applied (total chromatographic run time 17 min, including column re-equilibration). Concentrations measured with both methods were in good agreement. Hence, we propose the use of guard column-MS/MS to analyse a large number samples in a very short time (semi-quantification), and apply the chromatographic analysis only to those samples with levels close to/higher than the concentrations equivalent to the safe maximum daily intakes of the parent compounds (confirmation). This double strategy (semi-quantification by guard column-MS/MS and confirmation-when needed-by UHPLC-MS/MS) implies important savings in time and money | ||
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Guard column | |
| 650 | 4 | |a Phthalate metabolites | |
| 650 | 4 | |a Tandem mass spectrometry | |
| 650 | 4 | |a Ultra(high)-performance liquid chromatography | |
| 650 | 4 | |a Urine | |
| 650 | 7 | |a Plasticizers |2 NLM | |
| 700 | 1 | |a Casas-Ferreira, Ana María |e verfasserin |4 aut | |
| 700 | 1 | |a Nogal Sánchez, Miguel Del |e verfasserin |4 aut | |
| 700 | 1 | |a Pérez Pavón, José Luis |e verfasserin |4 aut | |
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