Hainan Provincial Key Laboratory of Resources Conservation and Development of Southern Medicine & Hainan Branch of the Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Haikou 570311, China.
Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China.
Toxins (Basel). 2022 Oct 29;14(11):742. doi: 10.3390/toxins14110742.
Mycotoxins can occur naturally in a variety of agriculture products, including cereals, feeds, and Chinese herbal medicines (TCMs), via pre- and post-harvest contamination and are regulated worldwide. However, risk mitigation by monitoring for multiple mycotoxins remains a challenge using existing methods due to their complex matrices. A multi-toxin method for 22 mycotoxins (aflatoxin B, B, G, G, M, M; ochratoxin A, B, C; Fumonisin B, B, B; 15-acetyldeoxynivalenol, 3-acetyldeoxynivalenol, diace-toxyscirpenol, HT-2, T-2, deepoxy-deoxynivalenol, deoxynivalenol, neosolaniol, zearalenone, and sterigmatocystin) using centrifugation-assisted solid-phase extraction (SPE) clean-up prior to ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis for Arecae Semen and its processed products was developed and validated. Several experimental parameters affecting the extraction and clean-up efficiency were systematically optimized. The results indicated good linearity in the range of 0.1-1000 μg/kg ( > 0.99), low limits of detection (ranging from 0.04 μg/kg to 1.5 μg/kg), acceptable precisions, and satisfactory recoveries for the selected mycotoxins. The validated method was then applied to investigate mycotoxin contamination levels in and its processed products. The mycotoxins frequently contaminating were aflatoxins (AFs), and the average contamination level and number of co-occurring mycotoxins in the Arecae Semen slices (Binlangpian) were higher than those in commercially whole Arecae Semen and Arecae Semen Tostum (Jiaobinlang). Sterigmatocystin was detected in 5 out of 30 Arecae Semen slices. None of the investigated mycotoxins were detected in Arecae pericarpium (Dafupi). The results demonstrated that centrifugation-assisted SPE coupled with UHPLC-MS/MS can be a useful tool for the analysis of multiple mycotoxins in and its processed products.
真菌毒素可以在各种农产品中自然产生，包括谷物、饲料和中草药（TCM），通过收获前和收获后的污染进行调节，并在全球范围内受到监管。然而，由于其复杂的基质，使用现有方法监测多种真菌毒素仍然是一个挑战。本研究建立并验证了一种采用离心辅助固相萃取（SPE）净化，结合超高效液相色谱-串联质谱（UHPLC-MS/MS）分析方法，用于检测槟榔及其制品中 22 种真菌毒素（黄曲霉毒素 B1、B2、G1、G2、M1、M2；赭曲霉毒素 A、B、C；伏马菌素 B1、B2、B3；15-乙酰脱氧雪腐镰刀菌烯醇、3-乙酰脱氧雪腐镰刀菌烯醇、二醋酸赛曲菌素、HT-2 毒素、T-2 毒素、脱氧雪腐镰刀菌烯醇-3-葡萄糖苷、雪腐镰刀菌烯醇、新茄病镰刀菌烯醇、玉米赤霉烯酮和桔青霉素）的方法。系统优化了影响提取和净化效率的几个实验参数。结果表明，在所研究的浓度范围内（0.1-1000μg/kg），该方法具有良好的线性关系（r>0.99），低检测限（0.04-1.5μg/kg），可接受的精密度和令人满意的回收率。该方法随后用于调查槟榔及其制品中真菌毒素的污染水平。污染槟榔的真菌毒素主要为黄曲霉毒素（AFs），槟榔切片（冰榔片）中真菌毒素的平均污染水平和共存真菌毒素的数量均高于市售的整个槟榔和槟榔烤片（加宝片）。在 5 批槟榔切片中检测到桔青霉素。在槟榔果皮（大腹皮）中均未检测到上述真菌毒素。结果表明，离心辅助 SPE 结合 UHPLC-MS/MS 可作为分析槟榔及其制品中多种真菌毒素的有用工具。
