QuEChERS-超高效液相色谱-串联质谱法同时测定坚果中20种真菌毒素

Simultaneous determination of 20 kinds of mycotoxins in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  真菌毒素  坚果

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  mycotoxins  nuts

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法同时测定坚果中20种真菌毒素含量的分析方法。方法 粉碎后的样品加水稀释, 经乙腈溶液超声提取, 氯化钠和无水硫酸铵盐析后, 用C18吸附剂净化。色谱柱为ACQUITY BEH C18柱(100 mm×2.1 mm, 1.7 μm), 以0.05%甲酸水溶液和乙腈为流动相梯度洗脱, 在电喷雾离子源正、负离子切换扫描模式下, 采用多反应监测模式进行检测, 外标法进行定量。结果 在相应的质量浓度范围内, 20种真菌毒素均呈现良好线性关系, 相关系数均大于0.992, 检出限和定量限分别为0.03~2.25 μg/kg和0.11~7.50 μg/kg。在不同基质中加入低、中、高3个添加水平, 平均加标回收率为77.5%~114.9%, 相对标准偏差为1.0%~6.5% (n=6)。结论 本方法稳定、准确、灵敏、快速, 适用于不同坚果基质中多种真菌毒素的快速检测和分析确证。

英文摘要:

      Objective To establish a method for the simultaneous determination of 20 kinds of mycotoxins in different nuts by ultra performance liquid chromatography-tandem mass spectrometry combined with QuEChERS extraction. Methods After homogenization, the nut samples were ultrasonic extracted by acetonitrile solution after diluted with water, salted out with sodium chloride and anhydrous ammonium sulphate, and purified with C18 adsorbent. An ACQUITY BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used, with 0.05% formic acid aqueous solution-acetonitrile as mobile phase for gradient elution. In the electrospray ionization positive and negative ion switching scanning mode, the samples were analyzed by multiple reaction monitoring and quantified by external standard method. Results All the 20 kinds of mycotoxins showed good linear relationships in their respective mass concentration ranges, and the correlation coefficients were greater than 0.992. The limits of detection and limits of quantification were 0.03?2.25 μg/kg and 0.11?7.50 μg/kg, respectively. The average recoveries of 20 kinds of mycotoxins in different matrices at low, medium and high spiked levels were ranged from 77.5%?114.9% (n=6), with relative standard deviations in the range of 1.0%?6.5%. Conclusion This method is stable, accurate, sensitive and rapid, and suitable for the rapid detection and analysis of multi-mycotoxins in different nut substrates.