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采用气相色谱-串联质谱法(GC-MS/MS)进行自动样品前处理和分析,测定食用油中的 3-氯-1,2-丙二醇酯(MCPD 酯)和缩水甘油酯。

Automated sample preparation and analysis by gas chromatography tandem mass spectrometry (GC-MS/MS) for the determination of 3- and 2-monochloropropanediol (MCPD) esters and glycidol esters in edible oils.

机构信息

dtoLABS, Via Pozzuoli, 13C/13D, 30038, Spinea (VE), Italy.

Department of Cardiologic, Thoracic and Vascular Sciences, University of Padova, Via Giustiniani, 2, 35127, Padova, Italy.

出版信息

J Chromatogr A. 2021 Aug 2;1650:462253. doi: 10.1016/j.chroma.2021.462253. Epub 2021 May 14.

DOI:10.1016/j.chroma.2021.462253
PMID:34049252
Abstract

The potentially carcinogenic process contaminant 3- and 2-monochloropropanediol esters (2-MCPD and 3-MCPD esters) and glycidyl esters (GEs) are under study in refined oils and foodstuffs. Legislation set recommended total daily intake (TDI) for 3-MCPD of 0.8 µg/kg and as low as reasonably achievable (ALARA) for glycidol. Usually, the so far adopted method for the determination of these contaminants relay on numerous and time-consuming steps for sample preparation (AOCS methods) and on GC-MS detection. The obtained sensitivities and the number of processable samples are thus limited. In this optic, new reliable methods that allow for the fast and sensitive determination of these contaminants in edible oils may be considered an improvement of the overall strategy of tackling the problem. In this paper a new automated method for sample preparation and detection by GC-MS/MS is presented and validated. Data on sensitivity (LOD at 1.5, 2.2 and 3 ng/g for 3-MCPD, 2-MCPD, 3-MBPD (deriving from glycidol), respectively), linearity across low and high calibration ranges and precision showed to be fit-for-purposes. Finally, the methodology was applied to ten extra virgin oil samples and one sample of sunflower seeds oil.

摘要

研究人员正在精炼油和食品中检测具有潜在致癌性的污染物 3-单氯丙二醇酯(3-MCPD 酯)和 2-单氯丙二醇酯(2-MCPD 酯)以及缩水甘油酯(GEs)。法规规定 3-MCPD 的建议每日总摄入量(TDI)为 0.8μg/kg,而缩水甘油的可合理达到的最低水平(ALARA)为尽可能低。通常,迄今为止,用于测定这些污染物的方法依赖于样品制备的多个耗时步骤(AOCS 方法)和 GC-MS 检测。因此,获得的灵敏度和可处理样品的数量有限。从这个角度来看,可用于快速灵敏地测定食用油中这些污染物的新可靠方法可被视为解决问题的整体策略的改进。本文提出并验证了一种用于 GC-MS/MS 分析的新自动化样品制备和检测方法。灵敏度数据(LOD 分别为 1.5、2.2 和 3ng/g 时,3-MCPD、2-MCPD 和 3-MBPD(来自缩水甘油))、低和高校准范围内的线性度以及精密度均符合要求。最后,该方法学应用于十种特级初榨橄榄油样品和一种葵花籽油样品。

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