超高效液相色谱串联质谱法同时检测13种植物生长激素残留物

Simultaneous determination of 13 plant growth regulators residues by ultra performance liquid chromatography/tandem mass spectrometry

目的采用超高效液相色谱-三重四极杆质谱技术,建立促进农作物生长的13种植物生长激素残留的检测方法。方法样品加甲醇超声提取,离心净化后进样分析,分析物经C18色谱柱分离,以甲酸铵-乙腈溶液作为流动相梯度洗脱,在电喷雾正、负离子扫描、多反应监测模式下,外标法定量分析,同时探讨了前处理和仪器分析条件对检测的影响。结果13种常见植物生长调节剂在1~1000μg/L范围内,峰面积与质量浓度的线性关系良好;当添加浓度水平在50、100、500μg/kg时,13种植物生长调节剂的平均回收率为92.5%~103.5%,相对标准偏差(relative standard deviation,RSD)为1.7%~5.6%,检出限(limit of detection,LOD)为0.8~4.2μg/kg。结论本方法简化了样品前处理步骤,具有良好的可靠性和灵敏度,适于植物源性食品中植物生长激素的快速检验与分析。

Objective To establish a method for the detection of 13 kinds of plant growth hormone residues by ultra performance liquid chromatography-triple quadrupole mass spectrometry.Methods The samples were extracted by ultrasonic extraction with methanol and purified by centrifugation.The analytes were separated by C18 chromatographic column and eluted by ammonium formate-acetonitrile solution as mobile phase gradient.In the mode of electrospray positive and negative ion scanning and multi-reaction monitoring,the external standard method was used for quantitative analysis.The influence of pretreatment and instrumental analysis conditions on the detection was also discussed.Results The linear relationship of 13 plant growth regulators was good in the range of 1-1000μg/L between peak area and mass concentration.When the concentration levels were 50,100 and 500μg/kg,the average recoveries of 13 plant growth regulators were 92.5%-103.5%,the relative standard deviations(RSDs)was 1.7%-5.6%,and the limits of detection(LODs)was 0.8-4.2μg/kg.Conclusion This method simplifies the sample pretreatment procedure,has good reliability and sensitivity,and it is suitable for rapid detection and analysis of plant growth regulators in plant nutrients.