Martínez-Domínguez Gerardo, Romero-González Roberto, Garrido Frenich Antonia
Research Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL), University of Almería, Agrifood Campus of International Excellence, ceiA3, E-04120 Almería, Spain.
Research Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL), University of Almería, Agrifood Campus of International Excellence, ceiA3, E-04120 Almería, Spain.
Food Chem. 2016 Apr 15;197(Pt A):907-15. doi: 10.1016/j.foodchem.2015.11.070. Epub 2015 Nov 14.
A multi-class methodology was developed to determine pesticides and mycotoxins in food supplements. The extraction was performed using acetonitrile acidified with formic acid (1%, v/v). Different clean-up sorbents were tested, and the best results were obtained using C18 and zirconium oxide for green tea and royal jelly, respectively. The compounds were determined using ultra high performance liquid chromatography (UHPLC) coupled to Exactive-Orbitrap high resolution mass spectrometry (HRMS). The recovery rates obtained were between 70% and 120% for most of the compounds studied with a relative standard deviation <25%, at three different concentration levels. The calculated limits of quantification (LOQ) were <10 μg/kg. The method was applied to green tea (10) and royal jelly (8) samples. Nine (eight of green tea and one of royal jelly) samples were found to be positive for pesticides at concentrations ranging from 10.6 (cinosulfuron) to 47.9 μg/kg (paclobutrazol). The aflatoxin B1 (5.4 μg/kg) was also found in one of the green tea samples.
开发了一种多类别方法来测定食品补充剂中的农药和霉菌毒素。萃取使用用甲酸（1%，v/v）酸化的乙腈进行。测试了不同的净化吸附剂，分别使用C18和氧化锆对绿茶和蜂王浆取得了最佳结果。使用超高效液相色谱（UHPLC）与Exactive-Orbitrap高分辨率质谱（HRMS）联用测定这些化合物。在三个不同浓度水平下，所研究的大多数化合物的回收率在70%至120%之间，相对标准偏差<25%。计算出的定量限（LOQ）<10μg/kg。该方法应用于绿茶（10个）和蜂王浆（8个）样品。发现九个样品（八个绿茶样品和一个蜂王浆样品）含有农药，浓度范围为10.6（嗪草酮）至47.9μg/kg（多效唑）。在一个绿茶样品中还发现了黄曲霉毒素B1（5.4μg/kg）。
