QuEChERS-超高效液相色谱-串联质谱法测定食用菌中7种荧光增白剂

建立了QuEChERS-超高效液相色谱-串联质谱法(UPLC-MS/MS)测定食用菌中7种荧光增白剂残留量的检测方法.样品前处理采用QuEChERS方法, 食用菌样品用水浸润后, 以甲酸和乙腈提取目标物, C18填料、正丙基乙二胺(PSA)和MgSO4净化, C18色谱柱分离, 乙腈和0.1%甲酸梯度洗脱, 多反应监测(MRM)正离子模式扫描.在优化条件下, 7种荧光增白剂在一定质量浓度范围内线性关系良好, 相关系数均大于0.991, 方法检出限(S/N=3)在0.05~0.40 μg/kg之间, 定量低限(S/N≥10)在0.2~1.3 μg/kg之间, 方法的平均回收率在70.1%~109.2%之间.本方法具有操作简单快捷、灵敏度高等优点.

Simultaneous Determination of Seven Kinds of Fluorescent White Agents in Mushroom by QuEChERS-UltraPerformance Liquid Chromatography-Tandem Mass Spectrometry

A method based on QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of seven kinds of fluorescent white agent residues in mushroom.After mixing with 10 mL of water, the sample was extracted with acidified acetonitrile, cleaned up by C18, primary secondary amine (PSA) and MgSO4.The separation of seven kinds of fluorescent white agents was performed on a C18 column with a gradient elution of acetonitrile and 0.1% acidified water as mobile phase.The target compounds were detected by electrospray ionization mass spectrometry in positive ion mode with multi reaction monitoring (MRM).Under the optimum conditions, the method had good linear relationship in the determination of the seven kinds of fluorescent white agents in a certain concentration range, with correlation coefficients greater than 0.991.Moreover, the limits of detection (S/N=3) were 0.05-0.4 μg/kg, the limits of quantitation (S/N=10) were 0.2-1.3 μg/kg, and the average recoveries for seven kinds of fluorescent white agent residues in msushroom were 70.1%-109.2%.In comparison with previous methods, the new procedure has characteristics of simple sample preparation and higher sensitivity.