改进 QuEChERS-超高效液相色谱-串联质谱法测定绿茶中 16 种真菌毒素含量

Determination of 16 kinds of mycotoxins in green tea by improved 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  绿茶  真菌毒素

英文关键词:QuEChERS  UPLC-MS/MS  green tea  Mycotoxins

中文摘要:

      目的 建立一种改进QuEChERS 技术结合超高效液相色谱-串联质谱法（UPLC-MS/MS）用于检测绿茶中16种真菌毒素的方法。方法 本方法以1%甲酸乙腈作为提取溶剂，经涡旋或震荡提取后，使用 N-丙基乙二胺 （PSA）和十八烷基键合硅胶吸附剂（C18）作为净化材料净化后，经 ACQUITY BEH C18色谱柱（100 mm × 2.1 mm，1.7 ?m）实现分离，采用电喷雾正负离子电离方式（ESI±）、多反应监测（MRM）模式进行检测，基质匹配曲线外标法定量。结果 16种真菌毒素在相应浓度范围内呈良好的线性关系，相关系数（r）均大于 0.998，此方法的检出限（LOD）为 0.2-100.0 μg/kg，定量限（LOQ） 为 0.5-300.0 μg/kg。在 1、2、10 倍 定量限的加标水平下，16种真菌毒素的回收率范围为 74.4%-110.9%，相对标准偏差（RSD）值均小于5%。应用新建立的方法对 10 批次绿茶样品进行分析检测，结果在 2 批次样品中检出了黄曲霉毒素B2，1 批次样品中检出玉米赤霉烯酮。结论 该方法灵敏度好，准确度高，可作为绿茶中真菌毒素的日常监测的有效检测方法。

英文摘要:

      Objective In order to developed a method to determine 16 mycotoxins in green tea by QuEChERStechnique combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The green tea sample was extracted with 1% formic acid in acetonitrile, and then purified with N-propylethylenediamine (PSA) and octadecylsilyl silica gel (C18) as the clean-up packings. The sample was then analyzed on an ACQUITY BEH C18 column(100 mm × 2.1 mm, 1.7 μm) to achieve the separation, and detected in multiple reaction monitoring (MRM) mode and quantified by matrix matching curve external standard method. Results The results showed that the 16 mycotoxins demonstrated good linearity in the corresponded concentration ranges with the correlation coefficients (r) greater than 0.998 .The limits of detection (LODs) of the method was in the range of 0.2-100.0 μg/kg ，and the limits of quantification (LOQs) of the method was in the range of 0.5-300.0 μg/kg, respectively. The recoveries of the 16 mycotoxins ranged from 74.4% to 110.9% at 1, 2 and 10 times LOQs spiked levels with relative standard deviations less than 5%. 10 batches of green tea samples were analysed and tested by this method and ATFB2 was detected in 2 batches and ZEN was detected in 1 batches. Conclusion The method is sensitive, accurate, and effective for routine monitoring of mycotoxins in green tea.