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建立经济高效的超快速液相色谱-串联质谱法用于微量分析何首乌中的多类真菌毒素。

Development of an economic ultrafast liquid chromatography with tandem mass spectrometry method for trace analysis of multiclass mycotoxins in Polygonum multiflorum.

机构信息

Pharmacy College, Jinzhou Medical University, Jinzhou, P. R. China.

Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing, P. R. China.

出版信息

J Sep Sci. 2019 Jan;42(2):491-500. doi: 10.1002/jssc.201800602. Epub 2018 Dec 11.

DOI:10.1002/jssc.201800602
PMID:30462887
Abstract

Rapid, economic, and highly effective determination of multiple mycotoxins in complex matrices has given huge challenges for the analytical method. In this study, an economic analytical strategy based on sensitive and rapid ultrafast liquid chromatography coupled to hybrid triple quadrupole/linear ion trap mass spectrometry technique was developed for the determination of seven mycotoxins of different chemical classes (aflatoxin B , B , G , and G , ochratoxin A, T-2 toxin, and HT-2 toxin) in Polygonum multiflorum. Target mycotoxins were completely extracted using a modified quick, easy, cheap effective, rugged, and safe method without additional clean-up steps. The types of extraction solvents and adsorbents for the extraction procedure were optimized to achieve high recoveries and reduce coextractives in the final extracts. Due to significant matrix effects for all analytes (≤68.9% and ≥110.0%), matrix-matched calibration curves were introduced for reliable quantification, exploring excellent linearity for the seven mycotoxins with coefficients of determination >0.9992. The method allowed high sensitivity with limit of detection in the range of 0.031-2.5 μg/kg and limit of quantitation in the range of 0.078-6.25 μg/kg, as well as satisfactory precision with relative standard deviations lower than 8%. Recovery rates were between 74.3 and 119.8% with relative standard deviations below 7.43%. The proposed method was successfully applied for 24 batches of P. multiflorum samples, and six samples were found to be positive with aflatoxin B , B , G , or ochratoxin A. The method with significant advantages, including minimum analytical time, low time and solvent consumption, and high sensitivity, would be a preferred candidate for economic analysis of multiclass mycotoxins in complex matrices.

摘要

在复杂基质中快速、经济、高效地测定多种真菌毒素给分析方法带来了巨大的挑战。本研究建立了一种基于灵敏、快速的超快速液相色谱与混合三重四极杆/线性离子阱质谱联用技术的经济分析策略,用于测定不同化学类别的 7 种真菌毒素(黄曲霉毒素 B 1 、B 2 、G 1 、G 2 、赭曲霉毒素 A、T-2 毒素和 HT-2 毒素)在何首乌中的含量。目标真菌毒素采用改良的快速、简便、廉价、有效、耐用、安全的方法完全提取,无需额外的净化步骤。优化了提取过程中的提取溶剂和吸附剂的类型,以获得高回收率并减少最终提取物中的共提取物。由于所有分析物的基质效应显著(≤68.9%和≥110.0%),因此引入基质匹配校准曲线进行可靠定量,探索了七种真菌毒素的优异线性关系,决定系数均大于 0.9992。该方法具有较高的灵敏度,检测限范围为 0.031-2.5μg/kg,定量限范围为 0.078-6.25μg/kg,相对标准偏差低于 8%,精密度良好。回收率在 74.3-119.8%之间,相对标准偏差低于 7.43%。该方法成功应用于 24 批何首乌样品,发现 6 批样品中存在黄曲霉毒素 B 1 、B 2 、G 1 或赭曲霉毒素 A。该方法具有显著优势,包括最短的分析时间、最低的时间和溶剂消耗以及高灵敏度,将成为复杂基质中多类真菌毒素经济分析的首选方法。

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