HPLC-MS/MS法测定水果中残留的多效唑和烯效唑

【目的】建立测定水果中2种植物生长延缓剂多效唑和烯效唑残留的高效液相色谱-电喷雾串联质谱分析方法。【方法】以甲醇为提取溶剂,采用超声波辅助溶剂萃取法萃取。以Waters Hypersil BDS C18色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。考察了流动相组分和流动相添加剂对质谱离子化效率的影响。【结果】多效唑和烯效唑在1.0~200.0μg/L线性关系良好(r>0.99),在2.0、10.0和50.0μg/kg的添加水平下,2种目标化合物的平均加标回收率为87%~103%,相对标准偏差小于5.0%,方法的检出限分别为1.5和2.0μg/kg。【结论】该方法具有检出限低、灵敏度高、选择性好、前处理方法简单、回收率高等优点,适用于水果中多效唑和烯效唑的残留检测。

Determination of Paclobutrazol and Uniconazole in Fruit by HPLC-MS/MS

【Objective】A comprehensive analytical method has been developed based on high liquid chromatography-electrospray ionization tandem mass spectrometry with positive ionization mode for determining paclobutrazol and uniconazole.【Method】Samples were extracted by methanol with ultrasonic wave assistant extraction(UAE).The reconstituted samples solution were analyzed by HPLC-MS/MS under positive ion mode,with Waters Hypersil BDS C18 column as the separate column.Effects of mobile phase and additives on ionization were assessed.【Result】The linear range was 1.0～200.0 μg/L,the correlation coefficients(r) were 0.999 0 and 0.998 9.Recoveries for the paclobutrazol and uniconazole ranged from 87% to 103% and the relative standard deviations were below 5.0% at the spiked level of 2.0,10.0 and 50.0 μg/kg.The detection limits of the method were 1.5 μg/kg and 2.0 μg/kg.【Conclusion】This method is sensitive and selective,and has low detection limit,high recovery range,and simple sample pre-treatment method.This method could be used to determine residual paclobutrazol and uniconazole in fruit.