Eom Taeyong, Cho Hyun-Deok, Kim Junghyun, Park Mihee, An Jinyoung, Kim Moosung, Kim Sheen-Hee, Han Sang Beom
a Department of Pharmaceutical Analysis, College of Pharmacy , Chung-Ang University , Dongjak-gu , Seoul , Republic of Korea.
b Food Contaminants Division, Department of Food Safety Evaluation , National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety , Cheongju-si , Chungcheongbuk-do , Republic of Korea.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2017 Nov;34(11):2011-2022. doi: 10.1080/19440049.2017.1363416. Epub 2017 Aug 14.
A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B, B, G and G; fumonisins B, B and B; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.
建立了一种使用液相色谱串联质谱法（LC-MS/MS）同时测定食用油中11种霉菌毒素的简单快速方法，这些霉菌毒素包括黄曲霉毒素B₁、B₂、G₁和G₂；伏马毒素B₁、B₂和B₃；赭曲霉毒素A；玉米赤霉烯酮；脱氧雪腐镰刀菌烯醇；以及T-2毒素。在本研究中，考察了QuEChERS（快速、简便、廉价、有效、耐用和安全）、结合分散液液微萃取的QuEChERS以及溶剂萃取法用于样品制备。在这些方法中，用甲酸/乙腈（5/95，v/v）混合物进行的溶剂萃取成功提取了所有目标霉菌毒素。随后，采用正己烷脱脂工艺去除食用油样品中的脂肪。质谱分析采用电喷雾电离，在极性切换模式下进行多反应监测。参照欧盟委员会法规（EC）401/2006，通过评估特异性、线性、回收率、定量限（LOQ）、准确度和精密度对所建立的LC-MS/MS方法进行了验证。除了定量限范围为0.025 ng/g至1 ng/g外，霉菌毒素回收率达到了51.6%至82.8%。事实证明，食用油是相对简单的基质，所建立的方法应用于9种食用油样品，包括大豆油、玉米油和米糠油，以评估潜在的霉菌毒素污染。检测水平显著低于国际监管标准。因此，我们预计基于简单的两步样品制备过程所建立的方法将适用于食用油中霉菌毒素污染的大规模筛查。
