Determination of multi-class pesticide residue in dietary supplements from grape seed extracts by ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry

• Published in: Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment Vol. 31; no. 9; pp. 1550 - 1561
• Main Authors: Nieto-García, Antonio José, Romero-González, Roberto, Garrido Frenich, Antonia
• Format: Journal Article
• Language: English
• Published: Abingdon Taylor & Francis 2014; Taylor & Francis Ltd
• Subjects: Berries; Biological and medical sciences; Chromatography; Chromatography, Liquid - methods; cyromazine; detection limit; Dietary supplements; diniconazole; ethyl acetate; Food Analysis - methods; Food industries; functional foods; Fundamental and applied biological sciences. Psychology; grape seed extract; Grape Seed Extract - chemistry; grape seeds; liquid chromatography; Mass spectrometry; Mass Spectrometry - methods; Matrix; pesticide residues; Pesticide Residues - chemistry; Pesticides; Pesticides - chemistry; Pesticides - classification; piperonyl butoxide; Reproducibility of Results; solid phase extraction; solvents; ultra-performance liquid chromatography; Vitaceae; Seeds; Fruit; Residue; Grape; grape seed extract; Pesticides; HPLC chromatography; dietary supplements; Liquid chromatography; Extract; Mass spectrometry; Food supplement; liquid chromatography; mass spectrometry; pesticides
• ISSN: 1944-0057; 1944-0049; 1944-0057
• DOI: 10.1080/19440049.2014.935489

A new method was developed and validated for the determination of multi-class pesticide residues in nutraceutical products obtained from grape seed extracts. The extraction procedure was based on QuEChERS methodology using ethyl acetate as solvent and a dispersive solid-phase extraction (dSPE) clean-up stage with C ₁₈ was included to minimise matrix effects. Pesticides determination was achieved using ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS); total running time was 11 min. Pesticides were quantified using matrix-matched calibration. The developed method was validated in terms of matrix effect, linearity, selectivity, limits of detection and quantification, trueness, repeatability and inter-day precision at three concentration levels (10, 50, 100 µg kg ⁻¹). Suitable recovery values were obtained for 76% of analysed pesticides at the lowest concentration (10 µg kg ⁻¹). For most of the compounds, relative standard deviation values were lower than 20% and 25% for intra- and inter-day precision, respectively. Finally, 106 pesticides were determined, and the method was applied to seven dietary supplements from grape seed extract, obtaining various positive results for piperonyl butoxide, cyromazine and diniconazole at concentrations ranging from 2.0 to 13.4 µg kg ⁻¹.