液相色谱-串联质谱法同时测定浆果类、瓜果类水果中19种植物生长调节剂的残留量

建立液相色谱-三重四级杆串联质谱法同时测定浆果类、瓜果类水果中19种植物生长调节剂残留量的检测方法。样品经优化的QuEChERS法进行前处理,用含1%乙酸的乙腈溶液提取,分散固相萃取净化,用Waters Acquity HSS T3色谱柱,乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱,采用电喷雾多反应监测模式,基质匹配标准溶液外标法定量。结果表明:19种植物生长调节剂在相应浓度范围内线性良好(r > 0.9902),该方法的检出限为0.09~16.8 μg/kg,定量限为0.27~50.4 μg/kg,加标回收率为69.4%~106.2%,RSD为1.1%~12.5%。随机检测200份样品,生长调节剂的检出率为6.3%。该方法灵敏度高,定性、定量准确,易于在实验室推广应用,可用于浆果类、瓜果类水果中的专属生长调节剂的测定。

Simultaneous Determination of 19 Kinds of Plant Growth Regulator Residues in Berries and Melons by Liquid Chromatography-Tandem Mass Spectrometry

To establish a method for the simultaneous determination of 19 plant growth regulators in berries and melons by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were pretreated by the quick, easy, cheap, effective, rugged and safe (QuEChERS) improved method.The plant growth regulator residues were extracted from the samples by acetonitrile (containing 1% acetic acid), cleaned up with QuEChERS and then analyzed using HPLC-MS/MS in multiple reaction monitoring (MRM) mode.The chromatographic analysis was carried out on a Waters Acquity HSS T3 column with acetonitrile and 0.1% formic acid solution as the mobile phases in gradient program, and quantified by matrix-matched external standard method. The results showed that, 19 kinds of plant growth regulators showed good linearity when they were in their concentration ranges (r > 0.9902). The limits of detection were within 0.09~16.8 μg/kg and the limits of quantification of the 19 plant growth regulators were within 0.27~50.4 μg/kg. The recoveries of 19 kinds of plant growth regulators were within 69.4%~106.2%, RSD was 1.1%~12.5%.Conclusion:The method was highly sensitive, qualitative and quantitative, easy to be used in the laboratory. It could be used to determine the specific growth regulators in berries and melons.