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采用液相色谱-串联质谱法和气相色谱-串联质谱法测定德国母乳样本中的草甘膦含量。

Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS.

作者信息

Steinborn Angelika, Alder Lutz, Michalski Britta, Zomer Paul, Bendig Paul, Martinez Sandra Aleson, Mol Hans G J, Class Thomas J, Pinheiro Nathalie Costa

机构信息

Federal Institute for Risk Assessment , Department of Pesticides Safety, Max-Dohrn-Strasse 8-10, 10589 Berlin, Germany.

RIKILT Wageningen UR, Natural Toxins and Pesticides, Akkermaalsbos 2, 6708 WB Wageningen, The Netherlands.

出版信息

J Agric Food Chem. 2016 Feb 17;64(6):1414-21. doi: 10.1021/acs.jafc.5b05852. Epub 2016 Feb 8.

DOI:10.1021/acs.jafc.5b05852
PMID:26808680
Abstract

This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For LC-MS/MS, sample preparation involved an ultrafiltration followed by chromatography on an anion exchange column. The analysis by GC-MS/MS involved an extraction step, cleanup on a cation exchange column, and derivatization with heptafluorobutanol and trifluoroacetic acid anhydride. Both methods were newly developed for breast milk and are able to quantify glyphosate residues at concentrations as low as 1 ng/mL. The methods were applied to quantify glyphosate levels in 114 breast milk samples, which had been collected from August to September of 2015 in Germany. The mothers participated at their own request and thus do not form a representative sample. In none of the investigated samples were glyphosate residues above the limit of detection found.

摘要

本研究描述了两种独立的分析方法用于测定母乳中草甘膦的验证和应用。它们分别基于液相色谱-串联质谱法(LC-MS/MS)和气相色谱-串联质谱法(GC-MS/MS)。对于LC-MS/MS,样品制备包括超滤,然后在阴离子交换柱上进行色谱分析。GC-MS/MS分析包括萃取步骤、在阳离子交换柱上净化以及用七氟丁醇和三氟乙酸酐衍生化。这两种方法都是专门为母乳新开发的,能够定量低至1 ng/mL浓度的草甘膦残留。这些方法被用于定量2015年8月至9月在德国采集的114份母乳样品中的草甘膦水平。母亲们是应自身要求参与的,因此不构成代表性样本。在所调查的样品中均未发现草甘膦残留超过检测限。

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