QuEChERS/超高效液相色谱-串联质谱技术同时测定食品中13种植物生长调节剂残留

Determination of plant growth regulators in food by QuEChERS and ultra performance liquid chromatography-tandem mass spectrometry

采用QuEChERS!超高效液相色谱-串联质谱技术同时测定食品中13种植物生长调节剂残留。样品经乙腈提取，分散固相萃取净化，以乙腈和2mmol／L甲酸铵溶液为流动相进行梯度洗脱，WatersC18色谱柱分离，采用电喷雾多反应监测模式，外标法定量。13种植物生长调节剂线性良好，线性相关系数均〉0．99，该方法的检出限在0．1～1．5μg／kg之间，定量限在0．3—5．0μg／kg之间。添加10、20和50μg／kg3个浓度水平，13种植物生长调节剂的平均回收率在75．9％-110．3％之间，相对标准偏差在0．1％-11．9％之间。将该技术应用于实际样品的测试，结果表明，方法简便、快速、灵敏度高，适用于食品中13种植物生长调节剂残留的同时测定。

An analysis method was established to determine plant growth regulators residues in food by QuEChERS and ultra performance liquid chromatography-tandem mass spec- trometry （UPLC/MS/MS）. The samples were extracted with acetonitrile and cleaned up with dispersive-solid phase extrac-tion. The target samples were separated by Waters Cls column with gradient elution using acetonitrile and 2 mmol/L ammo-niumformate as mobile phases. The samples were detected by tandem quadrupole mass spectrometry by multiple reaction monitoring （MRM）. External standard method was used to calibrate the results. The correlation coefficient was greater than 0.99. The limit of detection （LOD） was 0.1 - 1.5 μg/kg,and the limit of quantitation （LOQ） was 0. 3 - 5.0 μg/kg. The mean recoveries at the three spiked levels of 10 50 μg/kg were 75.9 -110.3%. The relative standard devia-tion （RSD） was 0.1-11.9%. The proposed method was successfully applied to the analysis of real samples. The sim-plicity ,sensitivity and good precision of the method made it well suitable for determination of plant growth regulators resi-dues in food.