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基于酸水解的 UPLC-MS/MS 法测定毒素的方法开发及其在茄科蔬菜及其制品中发生评估中的应用。

Development of Acid Hydrolysis-Based UPLC-MS/MS Method for Determination of Toxins and Its Application in the Occurrence Assessment in Solanaceous Vegetables and Their Products.

机构信息

Pesticide Safety Evaluation Research Center, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.

Key Laboratory for Safety Assessment (Environment) of Agricultural Genetically Modified Organisms, Ministry of Agriculture and Rural Affairs, Institute for Agro-Food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.

出版信息

Toxins (Basel). 2023 Mar 6;15(3):201. doi: 10.3390/toxins15030201.

Abstract

In this work, we proposed an acid hydrolysis-based analytical method for the detection of toxins (ATs) in solanaceous vegetables and their products with solid-phase extraction (SPE) and ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). This study was the first to reveal that some compounds in the eggplant matrix bind to altenusin (ALS). Validation under optimal sample preparation conditions showed that the method met the EU criteria, exhibiting good linearity (R > 0.99), matrix effects (-66.6--20.5%), satisfying recovery (72.0-107.4%), acceptable precision (1.5-15.5%), and satisfactory sensitivity (0.05-2 µg/kg for limit of detection, 2-5 µg/kg for limit of quantification). Out of 393 marketed samples, only 47 samples were detected, ranging from 0.54-806 μg/kg. Though the occurrence ratio (2.72%) in solanaceous vegetables could be negligible, the pollution status in solanaceous vegetable products was much more serious, and the incidences were 41.1%. In the 47 contaminated samples, the incidences were 4.26% for alternariol monomethyl ether (AME), 6.38% for alternariol (AOH) and altenuene (ALT), 42.6% for tentoxin (TEN), and 55.3% for tenuazonic acid (TeA).

摘要

本研究提出了一种基于酸水解的固相萃取-超高效液相色谱-串联质谱法,用于检测茄科蔬菜及其制品中的毒素(ATs)。这是首次发现茄子基质中的某些化合物与 alternusin(ALS)结合。在最佳样品制备条件下进行验证,该方法符合欧盟标准,表现出良好的线性(R > 0.99)、基质效应(-66.6--20.5%)、令人满意的回收率(72.0-107.4%)、可接受的精密度(1.5-15.5%)和良好的灵敏度(0.05-2 µg/kg 用于检测限,2-5 µg/kg 用于定量限)。在 393 个市售样品中,仅检测到 47 个样品,浓度范围为 0.54-806 µg/kg。虽然茄科蔬菜中的发生率(2.72%)可以忽略不计,但茄科蔬菜制品的污染状况更为严重,发生率为 41.1%。在 47 个受污染的样品中, alternariol monomethyl ether(AME)的发生率为 4.26%, alternariol(AOH)和 altenuene(ALT)的发生率为 6.38%, tentoxin(TEN)的发生率为 42.6%, tenuazonic acid(TeA)的发生率为 55.3%。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7759/10055482/8873f252d434/toxins-15-00201-g001.jpg

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