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采用液液萃取和低温净化的液相色谱-质谱联用技术分析牛奶中塑料材料潜在迁移物。

Analysis of potential migrants from plastic materials in milk by liquid chromatography-mass spectrometry with liquid-liquid extraction and low-temperature purification.

作者信息

Bodai Zsolt, Szabó Bálint Sámuel, Novák Márton, Hámori Susanne, Nyiri Zoltán, Rikker Tamás, Eke Zsuzsanna

机构信息

Joint Research and Training Laboratory on Separation Techniques (EKOL), Eötvös Loránd University , 1/A Pázmány Péter sétány, Budapest 1117, Hungary.

出版信息

J Agric Food Chem. 2014 Oct 15;62(41):10028-37. doi: 10.1021/jf503110v. Epub 2014 Oct 6.

Abstract

A simple and fast analytical method was developed for the determination of six UV stabilizers (Cyasorb UV-1164, Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, and Tinuvin 1577) and five antioxidants (Irgafos 168, Irganox 1010, Irganox 3114, Irganox 3790, and Irganox 565) in milk. For sample preparation liquid-liquid extraction with low-temperature purification combined with centrifugation was used to remove fats, proteins, and sugars. After the cleanup step, the sample was analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). External standard and matrix calibrations were tested. External calibration proved to be acceptable for Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, Irganox 3114, and Irganox 3790. The method was successfully validated with matrix calibration for all compounds. Method detection limits were between 0.25 and 10 μg/kg. Accuracies ranged from 93 to 109%, and intraday precisions were <13%.

摘要

开发了一种简单快速的分析方法,用于测定牛奶中的六种紫外线稳定剂(Cyasorb UV - 1164、Tinuvin P、Tinuvin 234、Tinuvin 326、Tinuvin 327和Tinuvin 1577)和五种抗氧化剂(Irgafos 168、Irganox 1010、Irganox 3114、Irganox 3790和Irganox 565)。样品制备采用低温纯化结合离心的液 - 液萃取法去除脂肪、蛋白质和糖分。净化步骤后,样品用高效液相色谱 - 串联质谱(LC - MS/MS)进行分析。测试了外标法和基质校准法。结果表明,外标法对Tinuvin P、Tinuvin 234、Tinuvin 326、Tinuvin 327、Irganox 3114和Irganox 3790是可接受的。该方法通过基质校准对所有化合物进行了成功验证。方法检测限在0.25至10μg/kg之间。准确度范围为93%至109%,日内精密度<13%。

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