建立基于 QuEChERS 的 UHPLC-MS/MS 法同时测定葡萄中 6 种毒素
Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Toxins in Grapes.
机构信息
Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.
College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China;.
出版信息
Toxins (Basel). 2019 Feb 1;11(2):87. doi: 10.3390/toxins11020087.
A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography⁻tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six toxins. After validation by determining the linearity (² > 0.99), recovery (77.8⁻101.6%), sensitivity (limit of detection in the range of 0.03⁻0.21 μg kg, and limit of quantification in the range of 0.09⁻0.48 μg kg), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10⁻1.64 μg kg, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the toxins contamination in grapes in China.
建立了超高效液相色谱-串联质谱法（UHPLC-MS/MS）同时测定葡萄中 alternariol（AOH）、altenuene（ALT）、tentoxin（TEN）、altenusin（ALS）、 tenuazonic acid（TeA）和 alternariol monomethyl ether（AME）的简单可靠分析方法。采用改良的 QuEChERS（快速、简单、廉价、有效、耐用和安全）方法，用乙腈提取，经氯化钠（0.5 g）和无水硫酸镁（0.5 g）净化，回收六种毒素。通过测定线性（²＞0.99）、回收率（77.8-101.6%）、灵敏度（检测限在 0.03-0.21 μg kg 范围内，定量限在 0.09-0.48 μg kg 范围内）和精密度（相对标准偏差（RSD）≤12.9%）对方法进行验证后，成功应用于揭示葡萄中毒素的污染状况。在 56 个葡萄样品中，有 40 个（占 71.4%）样品受到毒素污染。TEN 是最常发现的霉菌毒素（37.5%），浓度范围为 0.10-1.64 μg kg，其次是 TeA（28.6%）和 AOH（26.8%）。一些样品中也检测到 ALT（10.7%）、AME（3.6%）和 ALS（5.4%）。据我们所知，这是中国首次报道葡萄中存在这些毒素。
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