超高效液相色谱-串联质谱技术同时分析食品中多种植物激素残留

Determination of Plant Hormones Residues in Food by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立食品中多种植物激素残留量检测的超高效液相色谱-串联质谱的分析方法。[方法]样品经甲醇-水(体积比90∶10)提取,浓缩后经WCX小柱净化,采用Waters C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。[结果]在1～100μg/L的质量浓度范围内,各种植物激素相关系数均大于0.997,该方法的检出限在0.3～0.5μg/kg之间,定量限在1.0～1.5μg/kg之间。添加水平5～20μg/kg范围内,7种植物激素的回收率在80.2%～119.3%之间,日内和日间相对标准偏差在0.65%～7.28%之间。[结论]该方法简单、灵敏度高、分析时间短,适用于多种植物激素的测定。

A method was established for determining plant hormones residues in food by ultra performance liquid chromatography-tandem mass spectrometry（UPLC/MS/MS）. [Methods] The samples were extracted with methanol- water （90 ： 10, by vol）, and cleaned up by WCX cartridge. The target analytes were separated by Waters C18 column with gradient elution using acetonitrile and 0.1% formate in water as mobile phases. Positive electrospray ionization with multiple reaction monitoring mode was used in the detection. External standard method was used to determine the results. [Results] In the linear range（1-100 μg/L） of each plant hormones, the correlation coefficient was greater than 0.997 for each plant hormones. The limit of detection （LOD） were 0.3-0.5 μg/kg, and the limit of quantitation （LOQ） were 1.0-1.5 μg/kg. In the range of 5-20 μg/kg, the corresponding recoveries were 80.2-119.3%. The relative standard deviation （RSD） of intra-day and inter-day were 0.65-7.28%. [Conclusions] The simplicity, sensitivity and good precision of the method made it be well suitable for determination of plant hormones residues in food.