HPLC-MS/MS法测定水果中残留的多效唑和烯效唑

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

[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／k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。

[ 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 ClS 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.