National Research Council of Italy, Institute of Sciences of Food Production, Bari, Italy.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2011 Oct;28(10):1424-37. doi: 10.1080/19440049.2011.593192. Epub 2011 Jul 12.
A liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for the simultaneous determination of aflatoxins (B(1), B(2), G(1), G(2)), ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in wheat flour, barley flour and crisp bread was developed. Mycotoxin fragmentation patterns obtained by high-energy collision dissociation (HCD) were investigated to obtain quantitative and confirmatory information (two characteristic masses per mycotoxin) using Orbitrap™-based high-resolution mass spectrometry. LC-HRMS (full-scan) detection carried out by HCD allows the monitoring of the pseudo-molecular ion and an additional characteristic fragment (for each mycotoxin) with mass accuracy in the range 0.1-3.9 ppm, meeting current European regulatory requirements for LC-MS confirmatory analysis. A sample preparation procedure based on polymeric solid-phase extraction cartridges was applied, allowing recoveries higher than 74% for nine mycotoxins, with a relative standard deviation lower than 13%. Detection limits in the range 0.5-3.4 µg kg(-1) were obtained for three cereal matrices. A critical comparison between the proposed method and a validated method based on triple quadrupole mass spectrometry showed similar performance in terms of detection limits, recoveries and repeatability, and matrix effects. Based on an efficient sample extraction and clean-up, the LC-HCD-HRMS method reported here represents a reliable and robust alternative tool for mycotoxin analysis in food matrices as compared with well-established triple quadrupole-based approaches.
建立了一种同时测定小麦粉、大麦粉和脆饼中黄曲霉毒素（B(1)、B(2)、G(1)、G(2)）、赭曲霉毒素 A、脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮、T-2 和 HT-2 毒素的液相色谱-高分辨质谱（LC-HRMS）方法。采用高能碰撞解离（HCD）获得真菌毒素的碎片模式，利用基于轨道阱的高分辨质谱获得定量和确证信息（每种真菌毒素两个特征质量）。LC-HRMS（全扫描）通过 HCD 进行检测，允许监测准分子离子和另外一个特征碎片（每种真菌毒素一个），质量精度在 0.1-3.9 ppm 范围内，满足当前欧洲法规对 LC-MS 确证分析的要求。应用基于聚合物固相萃取小柱的样品制备程序，使得 9 种真菌毒素的回收率高于 74%，相对标准偏差低于 13%。在三种谷物基质中，检测限在 0.5-3.4 µg kg(-1)范围内。与基于三重四极杆质谱的验证方法进行了严格比较，在检测限、回收率和重复性以及基质效应方面，两种方法的性能相似。与基于成熟的三重四极杆的方法相比，本研究报告的 LC-HCD-HRMS 方法基于高效的样品提取和净化，是一种可靠且强大的替代工具，可用于食品基质中的真菌毒素分析。
