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

目的建立一种改进QuEChERS法结合超高效液相色谱-串联质谱法用于检测绿茶中16种真菌毒素的方法。方法本研究以1%甲酸乙腈作为提取溶剂,经涡旋或振荡提取后,使用N-丙基乙二胺和十八烷基键合硅胶吸附剂作为净化材料净化后,经ACQUITY BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)实现分离,采用电喷雾正负离子电离方式、多反应监测模式进行检测,基质匹配曲线外标法定量。结果在一定浓度范围内,16种真菌毒素均呈良好的线性关系,相关系数大于0.998,该方法的检出限在0.2~100.0μg/kg之间,定量限在0.5~300.0μg/kg之间。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在74.4%~110.9%之间,其相对标准偏差值均小于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AFB2,1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。

Objective To develop a method for the determination of 16 kinds of mycotoxins in green tea by improved QuEChERS technique combined with ultra performance liquid chromatography-tandem mass spectrometry.Methods The samples of green tea were extracted acetonitrile containing 1%formic acid and purified by purification materials containing octadecylsilyl silica gel and N-propylethylenediamine.The sample was then analyzed on an ACQUITY BEH C18 column(100 mm×2.1 mm,1.7μm)to achieve the separation,and detected in multiple reaction monitoring mode and quantified by matrix matching curve external standard method.Results Within a certain concentration range,the 16 kinds of mycotoxins revealed satisfactory linearities,with the correlation coefficients between 0.9985 and 0.9999.The limits of detection of the method were in the range of 0.2–100.0μg/kg,and the limits of quantification of the method were in the range of 0.5–300.0μg/kg.The recoveries of the 16 kinds of mycotoxins ranged from 74.4%to 110.9%at 1,2 and 10 times limit of quantitation spiked levels with relative standard deviations less than 5%.The 10 batches of green tea samples were analysed and tested by this method and AFB2 was detected in 2 batches and zearalenone was detected in 1 batches.Conclusion The method is sensitive,accurate,and effective for routine monitoring of mycotoxins in green tea.