分散固相萃取-超高效液相色谱-串联质谱法同时测定植物饮料中的8种磺酰脲类除草剂

Simultaneous Determination of Eight Sulfonylurea Herbicides in Plant Beverages by Dispersive Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

目的:建立同时测定植物饮料中8种磺酰脲类除草剂的超高效液相色谱-串联质谱法(Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry,UPLC-MS/MS)。方法:样品经乙腈提取,盐析分层,高速离心后,乙腈相使用C_(18)和Al-N固相萃取剂进行联合净化,最后经Poroshell120 EC-C_(18)(150 mm×3.0 mm,2.7μm)色谱柱洗脱分离,在电喷雾电离源正离子模式下进行离子化,采用多反应监测模式进行测定。结果:8种磺酰脲类除草剂的基质曲线在10~500μg·L^(-1)呈现良好线性关系,相关系数r^(2)均大于0.997。在添加浓度为10μg·kg^(-1)、20μg·kg^(-1)、50μg·kg^(-1)的条件下,8种磺酰脲类除草剂在乌龙茶和凉茶中的平均回收率为73.5%~88.8%,相对标准偏差为2.69%~8.66%。方法检出限为3.0μg·kg^(-1),方法定量限为10.0μg·kg^(-1)。结论:该方法回收率高,重现性好,且操作简单,可满足植物饮料中的8种磺酰脲类除草剂残留量的测定。

Object:An ultra performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of eight sulfonylurea herbicides in plant beverages.Method:Samples were extracted with acetonitrile and then salted out and layered.After high-speed centrifugation,acetonitrile phase was jointly purified with using C_(18)and Al-N solid-phase extraction agents.Finally,through Poroshell120 EC-C_(18)(150 mm×3.0 mm,2.7μm)chromatographic column elution separation,then ionized in positive ion mode of electric spray ionization source and determined in multiple reaction monitoring mode.Result:The matrix curves of 8 sulfonylurea herbicides ranged from 10~500μg·L^(-1)showed good linear relationships with the correlation coefficient r^(2)were both greater than 0.997.Under the conditions of spiked concentrations of 10μg·kg^(-1),20μg·kg^(-1),and 50μg·kg^(-1),the average recovery rates of 8 sulfonylurea herbicides in oolong tea and herbal tea were 73.5%~88.8%,while the relative standard deviations were 2.69%~8.66%.Moreover,the limit of detection of the method were both 3.0μg·kg^(-1)and the limit of quantification of the method were both 10.0μg·kg^(-1).Conclusion:The method had high recovery rate,good reproducibility and simple operation,which could satisfied the determination of 8 sulfonylurea herbicide residues in plant beverages.