液质联用法测定蔬果中12种植物生长调节剂

Determination of plant growth regulator residues in vegetables and fruits by liquid chromatography tandem mass spectrometry

目的建立蔬菜水果中赤霉素等12种植物生长调节剂残留的超高效液相色谱串联质谱法。方法样品经Qu ECh ERS法进行前处理,选用1%(V/V)乙酸的乙腈溶液提取,加无水硫酸镁和C18粉末净化,经C18反相色谱柱分离待测物,采用鞘流电喷雾离子化,正负离子分段扫描和多反应监测(MRM)模式检测,空白基质配置标准工作曲线,外标法定量。结果 12种植物生长调节剂在各自浓度范围内线性关系良好,相关系数均大于0.99;在3个不同添加水平下,空白基质青瓜的加标回收率为62.6%~94.4%,相对标准偏差低于6.27%;并用所建方法研究了89批次蔬菜水果中该12种植物生长调节剂的残留情况,结果满意。结论该方法操作简便、耗时短、有机试剂使用量少、灵敏度高、稳定性好,应用于日常的蔬菜水果中植物生长调节剂的检测可大大降低检测成本,缩短检测周期,具有实际应用价值。

Objective To establish a method to determine 12 plant growth regulator（ PGR） residues in vegetables and fruits by liquid chromatography tandem mass spectrometry（ UPLC-MS/MS） method. Methods The samples were initially extracted with acetonitrile containing 1%（ V/V） acetic acid,followed by cleaning-up using the powder of anhydrous magnesium sulfate and C18. The resulting samples were separated on a C18 reversed-phase chromatographic column,and detected under positive and negative multiple reactions monitoring（ MRM） mode through polarity switching between time segments. The matrix-matched external standard calibration curves were used for quantitative analysis. Results The calibration curves showed good linearity in each range with correlation coefficients greater than 0. 99. The recoveries of 12 PGRs spiked in cucumber samples at three levels ranged from 62. 6% to 94. 4%,with the relative standard deviations（ RSDs） less than 6. 27%. The established method was applied in determining the 12 PGRs in 89 batches of fruits and vegetables with satisfactory results. Conclusion This method is simple,time-saving and environmental friendly with high sensitivity and good reproducibility,having practical application value for its low-cost and short-circle.