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在线固相萃取-质谱联用避免色谱步骤可靠测定谷物类婴儿食品中的托烷生物碱

Reliable determination of tropane alkaloids in cereal based baby foods coupling on-line spe to mass spectrometry avoiding chromatographic step.

机构信息

Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.

Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.

出版信息

Food Chem. 2019 Mar 1;275:746-753. doi: 10.1016/j.foodchem.2018.09.137. Epub 2018 Sep 24.

Abstract

Cereal based foods are a major part of the infant diet and they can be contaminated with Solanaceae and other plants containing tropane alkaloids. This study was focused on the optimisation of an extraction procedure based on a solid-liquid method and an online SPE system, directly coupled to different mass spectrometry analysers as Orbitrap and triple quadrupole (QqQ), removing the chromatographic separation step. Total running analysis time was 15.8 min (17.3 min in the QqQ system). The developed method was validated obtaining recoveries ranging from 66 to 98% and 68-97% for the Orbitrap and QqQ respectively (RSD lower than 14.3%) and limits of quantification from 0.5 to 5 µg kg and 0.5-10 µg kg for the QqQ and Orbitrap analyser respectively. The validated method was applied to several cereal based baby food samples, finding a positive sample containing atropine (11.5 µg kg), scopolamine (2.8 µg kg) and apoatropine (7.5 µg kg).

摘要

谷物类食品是婴儿饮食的重要组成部分,它们可能受到茄科植物和其他含有托烷生物碱的植物的污染。本研究专注于优化一种基于固液萃取法和在线 SPE 系统的提取方法,该系统直接与不同的质谱分析仪(如 Orbitrap 和三重四极杆(QqQ))相连接,省去了色谱分离步骤。总分析时间为 15.8 分钟(QqQ 系统为 17.3 分钟)。所开发的方法经过验证,得到的回收率范围分别为 66-98%和 68-97%,适用于 Orbitrap 和 QqQ (RSD 低于 14.3%),定量限范围分别为 0.5-5μg/kg 和 0.5-10μg/kg,适用于 QqQ 和 Orbitrap 分析仪。该验证方法应用于几种基于谷物的婴儿食品样品,发现一个阳性样品含有阿托品(11.5μg/kg)、东莨菪碱(2.8μg/kg)和无托品碱(7.5μg/kg)。

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