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<p>This paper reports on the development of an analytical method for the simultaneous determination of 4-methyl phenol, 4-hydroxybenzoic acid and five bile acids, namely cholic acid, glycochenodeoxycholic acid, chenodeoxycholic acid, deoxycholic acid, and hyodeoxycholic acid (logP 1.6–4.9) in urine, exploring porous acrylic polymers as unconventional solid-phase extraction sorbents before HPLC-MS/MS analysis. These materials, obtained by polymerization of high internal phase emulsions with different composition, were used in a miniaturized setting (µSPE), preliminarily in synthetic urine samples enriched with 200&#xa0;ng&#xa0;mL<sup>−1</sup> of each selected compound. It was found that the polyethylene glycol (PEG)-modified polymer combines good analytical performance, in terms of extraction efficiency (76–100% for most analytes), from 1&#xa0;mL samples and single-fraction elution in pure ethanol. Recovery was assessed in untreated real urine (1&#xa0;mL, pH ~ 3.5) at three quality control levels (50, 200, 500&#xa0;ng&#xa0;mL<sup>−1</sup>) observing inter-day RSD below 20% (<i>n</i> = 3). The polymer exhibited a service life of at least ten sorption/desorption cycles, a further strength point of this sample treatment ascertained by greenness metrics. This streamlined procedure also provided satisfactory sample clean-up, with a negligible matrix-effect, as observed in HPLC-MS/MS. An ad hoc chromatographic method was developed to enable the simultaneous separation and quantification of all targets in a single run. Good linearity was observed in the range 10–600&#xa0;ng&#xa0;mL<sup>−1</sup> (R<sup>2</sup> &gt; 0.9919) with suitable sensitivity (a few ng mL<sup>−1</sup>) to future application for monitoring these endogenous compounds.</p> Graphical abstract <p></p>

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Quantification of gastric cancer biomarkers in the urine matrix by high internal phase emulsion polymer-based µsolid-phase extraction followed by HPLC-MS/MS

  • 期刊论文

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  • 发表日期：

    2026年5月4日

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  • Francesca Merlo,
  • Matteo Invernizzi,
  • Sofia Salerno,
  • Enrica Calleri,
  • Antonella Profumo,
  • Andrea Speltini

摘要

This paper reports on the development of an analytical method for the simultaneous determination of 4-methyl phenol, 4-hydroxybenzoic acid and five bile acids, namely cholic acid, glycochenodeoxycholic acid, chenodeoxycholic acid, deoxycholic acid, and hyodeoxycholic acid (logP 1.6–4.9) in urine, exploring porous acrylic polymers as unconventional solid-phase extraction sorbents before HPLC-MS/MS analysis. These materials, obtained by polymerization of high internal phase emulsions with different composition, were used in a miniaturized setting (µSPE), preliminarily in synthetic urine samples enriched with 200 ng mL−1 of each selected compound. It was found that the polyethylene glycol (PEG)-modified polymer combines good analytical performance, in terms of extraction efficiency (76–100% for most analytes), from 1 mL samples and single-fraction elution in pure ethanol. Recovery was assessed in untreated real urine (1 mL, pH ~ 3.5) at three quality control levels (50, 200, 500 ng mL−1) observing inter-day RSD below 20% (n = 3). The polymer exhibited a service life of at least ten sorption/desorption cycles, a further strength point of this sample treatment ascertained by greenness metrics. This streamlined procedure also provided satisfactory sample clean-up, with a negligible matrix-effect, as observed in HPLC-MS/MS. An ad hoc chromatographic method was developed to enable the simultaneous separation and quantification of all targets in a single run. Good linearity was observed in the range 10–600 ng mL−1 (R2 > 0.9919) with suitable sensitivity (a few ng mL−1) to future application for monitoring these endogenous compounds.

Graphical abstract