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Paniagua González, Gema

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  • Publicación
    Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS
    (Elsevier, 2024-04-09) Fernández Pintor, Begoña; Gañán Aceituno, Judith; Morante Zarcero, Sonia; Sierra, Isabel; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    Two homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.
  • Publicación
    On-line flow injection molecularly imprinted solid phase extraction for the preconcentration and determination of 1-hydroxypyrene in urine samples
    (Elsevier, 2017-05-01) Serrano, Montserrat; Bartolomé, Mónica; Gañán Aceituno, Judith; Gallego Picó, Alejandrina; Bravo Yagüe, Juan Carlos; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª
    New analytical strategies tend to automation of sample pre-treatment and flow analysis techniques provided a number of enhanced analytical methods allowing high throughput. Flow techniques are usually faster, more robust and more flexible than their batch equivalents. In addition, flow methods use less sample and reagent amounts and reduce analytical costs and waste. A flow injection solid-phase extraction pre-concentration system using a molecularly imprinted polymer (MIP) packed micro-column was developed for the determination of 1-hydroxypyrene in human urine with fluorescence detection. The pre-concentration of 1-hydroxypyrene on the MIP was carried out based on the specific retention of analyte by on-line introducing the sample into the micro-column system. Methanol and dichloromethane mixture was used to elute the retained analyte for fluorometric analysis. Important influencing factors were studied in detail, in batch and in flow (MISPE procedure optimisation, sample and eluent volumes, flow rate, dimensions of MIP micro-column and amounts of packing material, etc). To the best of our knowledge, this is the first on-line flow injection molecularly imprinted solid phase extraction for the pre-concentration and determination of hydroxylate PAH metabolite in urine samples. The optimised method was successfully applied to the determination of 1-Hydroxypyrene in spiked urine samples, with recoveries in the range of 74–85% and RSD<4.6%. Under optimum experimental conditions, the linearity concentration range used was 10–400 μg L−1, R2>0.996. We obtained limit of detection and quantification of 3.1 μg L−1 and 10.5 μg L−1, respectively
  • Publicación
    Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS
    (Elsevier, 2024-04-09) Fernández Pintor, Begoña; Gañán Aceituno, Judith; Morante Zarcero, Sonia; Garcinuño, Rosa María; Sierra, Isabel; Paniagua González, Gema; Fernández Hernando, Pilar
    Two homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.