超高效液相色谱-串联质谱法同时测定蜂花粉中10种真菌毒素

Determination of Ten Mycotoxins Residues in Bee Pollen by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

目的建立一种同时检测蜂花粉中10种真菌毒素的超液相色谱-串联质谱方法。方法蜂花粉经酸化的乙腈水溶液超声提取,经快速净化柱净化后,采用C_(18)色谱柱(2.1 mm×100 mm,2.7μm)分离,以乙腈和水为流动相,串联质谱电喷雾正离子源模式扫描,并采用多反应监测模式检测,采用基质匹配标准曲线进行定量分析。结果10种真菌毒素在各自的质量浓度范围内具有良好的线性关系,相关系数r均大于0.999,检出限范围在1~1.8μg/kg之间,10种真菌毒素3个添加水平下的回收率范围为71.3%~106.5%,相对标准偏差<10%。结论该方法快速高效,定量准确,可实现蜂花粉中多种真菌毒素的同时快速测定。

Objective To develop an analytical method using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the determination of fumonisin(FB1,FB2,FB3),aflatoxins(AFB1,AFB2,AFG1,AFG2)and ochratoxin(OTA,OTB,OTC)in bee pollen.Methods The analytes in the sample were ultrasonically extracted with a mixture of acetonitrile-water-formic acid solution,and followed by a QuEChERS method.Chromatographic separation of the ten mycotoxins was carried out on a C_(18) column(2.1 mm×100 mm,2.7μm)with acetonitrile and water as mobile phases of gradient elution.The mycotoxins were quantified using UPLC-MS/MS with an electrospray ionization(ESI)resource under positive mode and multiple reaction monitoring(MRM)mode was adopted.Matrix matched calibration standard curves were used for quantitative analysis to reduce the matrix effects.Results The 10 mycotoxins had good linear relationships in their respective mass concentration ranges.The correlation coefficients(r)of the mycotoxins were higher than 0.999.The limits of detection(LOD)of 10 mycotoxins were in the ranges of 1-1.8μg/kg.The recoveries at three levels were in the ranges of 71.3%-106.5%with RSDs less than 10%.Conclusion The method is fast,efficient,and quantitatively accurate,and can be successfully applied for the simultaneous and rapid determination of 10 mycotoxins in bee pollen.