UPLC-MS/MS法同时测定葡萄中4种植物生长调节剂研究

Determination of 4 Plant Growth Regulator Residues in Grape by UPLC-MS/MS

该文建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）同时测定葡萄中4种植物生长调节剂的方法。样品经乙腈提取,WAX小柱净化,采用BEH C18色谱柱分离,以乙腈和水为流动相进行梯度洗脱。采用电喷雾离子化,负离子分段扫描和多反应监测模式（MRM）检测,外标法定量。结果表明：赤霉素、对氯苯氧乙酸、氯吡脲、2,4-二氯苯氧乙酸在1~200ng/m L范围内线性关系良好,相关系数均大于0.990;4种植物生长调节剂的方法检出限均为0.2μg/kg,方法定量限为0.5μg/kg,样品添加回收试验的平均回收率为74.8%~101.5%,相对标准偏差为3.3%~8.6%（n=7）。该方法简单、灵敏度高、分析时间短,适用于葡萄中4植物生长调节剂的测定。

A method was established for determining 4 plant growth regulator residues in grapes by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）.Samples were extracted with acetonitrile, and cleaned up on a WAX cartridge.The target analytes were separated on a BEH C18 column with gradient elution using a mobile phase made up of acetonitrile and water.The samples were detected under negative multiple reactions moni- toring（MRM） mode through polarity switching between time segments.The result showed that the linearities of gibber- ellic acid, 4-chlorophenoxyaceticacid, forchlorfenuron, and 2, 4-dichlorophenoxyacetic were in the concentration range of lng/mL - 200ng/mL, with the correlation coefficients higher than 0.990.The limits of detection （LOD）and the limits of quantitation （LOQ）of the method were 0.2μg/kg and 0.5μg/kg.The average spiked recovery rates were in the range of 74.8% - 101.5%.The result showed that the relative standard deviation （RSD, n=7）was 3.3% - 8.6%. The method proved to be simple, sensitive, rapid and suitable for the determination of 4 plant growth regulator resi- dues in grapes.