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开发并验证了一种特定且灵敏的气相色谱-串联质谱法,用于检测大量食品中的双酚 A 残留。

Development and validation of a specific and sensitive gas chromatography tandem mass spectrometry method for the determination of bisphenol A residues in a large set of food items.

机构信息

LUNAM Université, Oniris, Laboratoire d'Etude des Résidus et Contaminants dans les Aliments (LABERCA), Nantes F-44307, France.

LUNAM Université, Oniris, Laboratoire d'Etude des Résidus et Contaminants dans les Aliments (LABERCA), Nantes F-44307, France.

出版信息

J Chromatogr A. 2014 Oct 3;1362:241-9. doi: 10.1016/j.chroma.2014.07.105. Epub 2014 Aug 19.

DOI:10.1016/j.chroma.2014.07.105
PMID:25200533
Abstract

BPA-containing products are widely used in foodstuffs packaging as authorized within the European Union (UE no. 10/2011). Therefore, foods and beverages are in contact with BPA which can migrate from food contact material to foodstuffs. An accurate assessment of the exposure of the consumers to BPA is crucial for a non-ambiguous risk characterization. In this context, an efficient analytical method using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS), in the selected reaction monitoring (SRM) mode, was developed for the quantification of BPA in foodstuffs at very low levels (<0.5μgkg(-1)). A standard operating procedure, based on the combination of two successive solid phase extractions (SPE), was developed for various liquid and solid foodstuffs. The use of (13)C12-BPA as internal standard allowed accurate quantification of BPA by isotopic dilution. Control charts based on both blank and certified materials have been implemented to ensure analytical data quality. The developed analytical method has been validated according to in-house validation requirements. R(2) was better than 0.9990 within the range [0-100μgkg(-1)], the trueness was 4.2%. Repeatability and within-laboratory reproducibility ranged from 7.5% to 19.0% and 2.5% to 12.2%, respectively, at 0.5 and 5.0μgkg(-1) depending on the matrices tested for. The detection and quantification limits were 0.03 and 0.10μgkg(-1), respectively. The reporting limit was 0.35μgkg(-1), taking into account the mean of the laboratory background contamination. The global uncertainty was 22.2% at 95% confidence interval.

摘要

含双酚 A 的产品被广泛用于食品包装,这在欧盟(欧盟第 10/2011 号)是被授权的。因此,食品和饮料会接触到双酚 A,而双酚 A 可能会从食品接触材料迁移到食品中。准确评估消费者接触双酚 A 的情况对于明确风险评估至关重要。在此背景下,开发了一种使用气相色谱-串联质谱(GC-MS/MS)、选择反应监测(SRM)模式的高效分析方法,可在极低水平(<0.5μgkg(-1))下定量食品中的双酚 A。基于两次连续固相萃取(SPE)的组合,开发了一种用于各种液体和固体食品的标准操作程序。使用(13)C12-BPA 作为内标,通过同位素稀释法可以准确地定量双酚 A。基于空白和认证材料的控制图已被实施,以确保分析数据的质量。所开发的分析方法已根据内部验证要求进行了验证。在 [0-100μgkg(-1)]范围内,R(2) 优于 0.9990,准确度为 4.2%。重复性和实验室内部再现性在 0.5 和 5.0μgkg(-1)时分别为 7.5%-19.0%和 2.5%-12.2%,具体取决于测试的基质。检测限和定量限分别为 0.03 和 0.10μgkg(-1)。报告限为 0.35μgkg(-1),考虑到实验室背景污染的平均值。在 95%置信区间内,总不确定度为 22.2%。

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