采用QuEChERS萃取结合混合模式固相萃取净化的超高效液相色谱-串联质谱法测定咖啡中的赭曲霉毒素A和伏马毒素

UHPLC-MS/MS determination of ochratoxin A and fumonisins in coffee using QuEChERS extraction combined with mixed-mode SPE purification.

作者信息

Nielsen Kristian Fog, Ngemela Archard Ferdinand, Jensen Lene Bai, de Medeiros Lívia Soman, Rasmussen Peter Have

机构信息

Department of Systems Biology, Technical University of Denmark , Building 221, 2800 Lyngby, Denmark.

出版信息

J Agric Food Chem. 2015 Jan 28;63(3):1029-34. doi: 10.1021/jf504254q. Epub 2015 Jan 16.

Abstract

A method was developed for simultaneous determination of the mycotoxins: ochratoxin A (OTA) and fumonisins B2 (FB2), B4 (FB4), and B6 (FB6) in green, roasted, and instant coffee. Extraction was performed by QuEChERS (quick, easy, cheap, effective, rugged, and safe) under acidic conditions followed by mixed-mode reversed phase-anion exchange solid phase extraction. OTA and FB2 were detected at levels down to 0.5 and 2 μg/kg by UHPLC-MS/MS and quantitated via isotope dilution using U-(13)C-labeled FB2 and OTA as internal standards. Mixing 20% isopropanol in the acetonitrile of the acidic UHPLC gradient system increased the signal intensity by 50% and decreased the ion-suppression with 50-75% in roasted coffee samples. About half of the roasted coffee samples (n = 57, from 9 countries) contained detectable levels of OTA, however, with only 5 samples above the EU regulatory limit of 5 μg/kg and the highest with 21 μg/kg. None of the 25 instant coffee samples contained OTA above the EU regulatory level of 10 μg/kg. Nonetheless, the toxin could be detected in 56% of the analyzed instant coffee samples. Fumonisins were not detected in any of the roasted or instant coffee samples (n = 82). However, in the green coffee samples (n = 18) almost half of the samples were positive with a maximum value of 164 μg/kg (sum of FB2, FB4, and FB6). This discrepancy between green coffee and processed coffees indicated that the fumonisins decompose during the roasting process, which was confirmed in roasting experiments. Here fumonisins could not be detected after roasting of the green, 164 μg/kg coffee, sample. Under the same conditions, OTA was reduced from 2.4 to 0.5 μg/kg.

摘要

开发了一种同时测定生咖啡、烘焙咖啡和速溶咖啡中霉菌毒素赭曲霉毒素A(OTA)以及伏马毒素B2(FB2)、B4(FB4)和B6(FB6)的方法。在酸性条件下通过QuEChERS(快速、简便、廉价、有效、耐用且安全)进行萃取,随后进行混合模式反相 - 阴离子交换固相萃取。通过超高效液相色谱 - 串联质谱法(UHPLC - MS/MS)检测到OTA和FB2的水平低至0.5和2 μg/kg,并以U-(13)C标记的FB2和OTA作为内标通过同位素稀释进行定量。在酸性UHPLC梯度系统的乙腈中混合20%的异丙醇,可使烘焙咖啡样品中的信号强度提高50%,并使离子抑制降低50 - 75%。约一半的烘焙咖啡样品(n = 57,来自9个国家)含有可检测水平的OTA,然而,只有5个样品超过欧盟5 μg/kg的监管限量,最高为21 μg/kg。25个速溶咖啡样品中没有一个含有超过欧盟10 μg/kg监管水平的OTA。尽管如此,在所分析的速溶咖啡样品中,56%可检测到该毒素。在任何烘焙咖啡或速溶咖啡样品(n = 82)中均未检测到伏马毒素。然而,在生咖啡样品(n = 18)中,几乎一半的样品呈阳性,最大值为164 μg/kg(FB2、FB4和FB6的总和)。生咖啡和加工咖啡之间的这种差异表明伏马毒素在烘焙过程中分解,这在烘焙实验中得到了证实。在此实验中,生咖啡样品(164 μg/kg)烘焙后未检测到伏马毒素。在相同条件下,OTA从2.4 μg/kg降至0.5 μg/kg。

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