Development and validation of a rapid and efficient method for simultaneous determination of mycotoxins in coix seed using one-step extraction and UHPLC-HRMS
Development and validation of a rapid and efficient method for simultaneous determination of mycotoxins in coix seed using one-step extraction and UHPLC-HRMS
复制标题
一步提取和 UHPLC-HRMS 快速有效同时测定薏苡仁中霉菌毒素的方法的开发和验证
DOI：
10.1080/19440049.2020.1833089
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发表时间：
2020-10-30
影响因子：
2.9
通讯作者：
Wang, Songxue
中科院分区：
文献类型：
--
作者：
Wu, Yu;Ye, Jin;Wang, Songxue
摘要薏苡仁是我国及亚洲各国的重要食品和中药。值得注意的是，薏苡仁目前在中国被用作治疗COVID-19的传统药物。然而，薏苡仁普遍受到霉菌毒素的污染，这种风险不容忽视。本文建立了一种直接提取和超高效液相色谱-高分辨质谱联用同时检测薏苡仁中24种真菌毒素的方法。优化了UHPLC-HRMS仪器和数据采集参数以及样品预处理。与三种商业化的固相萃取净化方法相比，一步萃取法具有操作简便、样品制备时间短、成本低、回收率高、基质效应好等优点。方法验证结果表明，所有真菌毒素均具有良好的线性和灵敏度。回收率在74.2- 101.1%之间，RSD在0.1- 5.8%之间。24种真菌毒素的LOQ范围为0.5-100 µg/kg。为了调查商业薏苡仁中这些真菌毒素的污染水平，从中国市场收集了70多个样品，并使用新开发的方法进行了分析。玉米赤霉烯酮（阳性率：98.7%，范围：1.1-1562 µg/kg）、脱氧雪腐镰刀菌烯醇（阳性比率：87%，范围：8.4-382.5 µg/kg）、雪腐镰刀菌烯醇（阳性比率：85.7%，范围：26.8-828.2 µg/kg）、伏马菌素B1（阳性比率：84.4%，范围：2.5-314.5 µg/kg）、伏马菌素B2（阳性比率：75.3%，范围：1.6-72.8 µg/kg）、伏马菌素B3（阳性比率：48%，范围：1.0-203.6 µg/kg）、黄曲霉毒素B1（阳性比率：29.9%，范围：0.39-14.7 µg/kg）、杂色曲霉素（阳性率：29.9%，范围：1.4-51.6 µg/kg）和细链偶氮酸（阳性率：19.5%，范围：36.1-105.7 µg/kg）是最常见的真菌毒素污染物。这些结果强调了常规监测和控制薏苡仁中真菌毒素的重要性。
ABSTRACT Coix seed is an important food and traditional Chinese medicine in China and other Asian countries. Notably, coix seed is currently being used as a traditional medicine for the treatment of COVID-19 in China. However, coix seeds are generally contaminated by mycotoxins, and this risk cannot be ignored. In this paper, we developed a method that involves direct extraction and UHPLC-HRMS analysis for the simultaneous detection of 24 mycotoxins in coix seeds. UHPLC-HRMS instrument and data acquisition parameters, and the sample pretreatment were optimised. One-step extraction showed several advantages compared to the three commercial solid-phase extraction clean-up methods, including ease of use, reduced time of sample preparation, low cost, good recovery, and acceptable matrix effect. The method validation results indicate that all mycotoxins have good linearity and sensitivity. Recoveries were between 74.2–101.1%, and RSD ranged from 0.1–5.8%. The LOQs for 24 mycotoxins were in the range of 0.5–100 µg/kg. To survey the contamination levels of these mycotoxins in commercial coix seeds, more than 70 samples were collected from Chinese markets and were analysed using the newly developed method. Zearalenone (positive ratio: 98.7%, range:1.1–1562 µg/kg), deoxynivalenol (positive ratio: 87%, range: 8.4–382.5 µg/kg), nivalenol (positive ratio: 85.7%, range: 26.8–828.2 µg/kg), fumonisin B1 (positive ratio: 84.4%, range:2.5–314.5 µg/kg), fumonisin B2 (positive ratio: 75.3%, range:1.6–72.8 µg/kg), fumonisin B3 (positive ratio: 48%, range:1.0–203.6 µg/kg), aflatoxin B1 (positive ratio: 29.9%, range: 0.39–14.7 µg/kg), sterigmatocystin (positive ratio: 29.9%, range: 1.4–51.6 µg/kg), and tenuazonic acid (positive ratio: 19.5%, range 36.1–105.7 µg/kg) were the most frequent mycotoxin contaminants. These results highlight the importance of routine monitoring and control of mycotoxins in coix seeds.