超高效液相色谱-串联质谱法测定果蔬汁类及其饮料中22种镰刀菌属毒素

目的 建立果蔬汁类及其饮料中22种镰刀菌属毒素的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测的实验方法。方法 样品经水和乙腈提取,QuEChERS净化,氮吹至近干,1 mL 80%乙腈水(体积分数)复溶,以乙腈和0.1%甲酸水(2mmol/L甲酸铵)为流动相,经ACQUITY UPLC CSH Phenyl-Hexyl 反相柱梯度分离,UPLC-MS/MS在正、负离子模式下多反应监测,基质配制外标法定量。结果 22种镰刀菌属毒素在线性范围内,相关系数平方(R2)均大于0.985,回收率在66.6%-119.1%之间,相对标准偏差在2.64%-14.96%之间。结论 该方法具有前处理方式简单、分析时间短、灵敏度好、准确度高、杂质干扰小等特点,可以用于果蔬汁类及其饮料中22种镰刀菌属毒素的检测。

Determination of 22 fusarium toxins in fruit and vegetable juices and beverages by High-performance liquid chromatography tandem mass spectrometry

ABSTRACT：Objective A ultra-high performance liquid chromatography-tandem mass spectrometry method was established for the detection of 22 Fusarium toxins in fruit and vegetable juices and their beverages. Methods The sample was extracted with water and acetonitrile, purified by QuEChERS, nitrogen blown to near dryness, and re dissolved in 1 mL of 80% acetonitrile water (volume fraction). Acetonitrile and a 0.1% formic acid aqueous solution containing 2 mmol/L ammonium formate were used as the mobile phase, and subjected to ACQUITY UPLC CSH Phenol Hexy reverse phase column gradient separation. UPLC-MS/MS was used for multi reaction monitoring in positive and negative ion modes, and the matrix was prepared using an external standard method for quantification. Results The results showed that 22 types of Fusarium toxins were within a linear range, with correlation coefficient squared (R2) greater than 0.985, recovery rates between 66.6% and 119.1%, and relative standard deviation between 2.64% and 14.96%. Conclusion This method has the characteristics of simple pre-treatment, short analysis time, good sensitivity, high accuracy, and low impurity interference. It can be used for the detection of 22 Fusarium toxins in fruit and vegetable juices and their beverages.