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HPLC-MS/MS法测定水果中残留的多效唑和烯效唑

         

摘要

[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 Iimit, high recovery range , and simple sample pre - treatment method . This method could be used to determine residual paclobutrazol and uniconazole in fruit .%[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]多效哇和烯效唑在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,适用于水果中多效哇和烯效哇的残留检测.

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