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

Determination of 22 kinds of Fusarium toxins in fruit and vegetable juices and beverages by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  果蔬汁类及其饮料  QuEChERS净化  超高效液相色谱串联质谱  镰刀菌属毒素

英文关键词:fruit and vegetable juices and beverages  QuEChERS purification  ultra performance liquid chromatography-tandem mass spectrometry  Fusarium toxin

中文摘要:

      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)检测的分析方法。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, 采用Waters ACQUITY UPLC CSH Phenyl-Hexyl反相色谱柱(100 mm×2.1 mm, 1.7 μm)梯度分离, 以乙腈和0.1%甲酸水(2 mmol/L甲酸铵)为流动相进行梯度洗脱, 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, 线性关系良好, 决定系数(R2)均大于等于0.985, 回收率在60.1%~119.7%之间, 相对标准偏差在2.64%~15.53%之间。结论 该分析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。

英文摘要:

      Objective To establish an analytical method for the detection of 22 kinds of Fusarium toxins in fruit and vegetable juices and their beverages using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with water and acetonitrile, purified by QuEChERS, blown to near dry with nitrogen, redissolved with 1 mL of 80% acetonitrile water (volume fraction), separated by gradient on Waters ACQUITY UPLC CSH Phynyl-Hexyl reverse phase chromatographic column (100 mm×2.1 mm, 1.7 μm), gradient eluted with acetonitrile and 0.1% formic acid water (2 mmol/L ammonium formate) as mobile phase, multi-reaction monitoring by UPLC-MS/MS in positive and negative ion modes, and matrix preparation external standard method quantitative. Results The 22 kinds of Fusarium toxins were within a linear range, with a good linear relationship. Coefficient of determination (R2) was greater than or equal to 0.985, and the recovery rates were between 60.1% and 119.7%. The relative standard deviations were between 2.64% and 15.53%. Conclusion This analysis 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 kinds of Fusarium toxins in fruit and vegetable juices and their beverages.