超高效液相/串联质谱法测定水中苯甲酰脲类农药残留

建立了固相萃取(SPE)-超高效液相色谱/大气压化学电离源/三重四极杆串联质谱(UPLC-MS/MS)同时测定水中7种苯甲酰脲类杀虫剂残留的方法。过滤后的样品经HLB固相萃取柱富集净化后,目标化合物经10 mL二氯甲烷洗脱并浓缩,1 mL甲醇定容后,采用BEH C18柱,以水(5 mmol/L乙酸铵)-乙腈作为流动相进行梯度洗脱,采用串联质谱作为检测器进行检测。7种苯甲酰脲类杀虫剂在相关线性范围内线性良好(r=0.999 1～0.999 5),回收率为71.8%～114%,相对标准偏差为3.3%～18.8%,方法检出限为7.0～16.0 ng/L。该方法快速,灵敏度高,适用于测定水体中7种苯甲酰脲类杀虫剂的残留。

Determination of Benzoylurea Insecticides Residues in Water by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for analysis of 7 benzoylurea insecticides residues in water was developed using solid phase extraction(SPE)and ultra-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry(UPLC-APCI/MS/MS).Water samples were extracted and cleaned by SPE through HLB column,and then BEH C18 column was used for separation,with a linear gradient elution program of acetonitrile-5 mmol/L aqueous ammonium acetate as the mobile phase.Multiple reaction monitoring(MRM)was used for selective detection of 7 benzoylurea insecticides.There were good linear relations(0.9991～0.9995)of all 7 benzoylurea insecticides.The recoveries ranged from 71.8% to 114%,with relative standard deviations of 3.3%～18.8% and detection limits between 7.0～16.0 ng/L.The method which is fast and sensitive is applicable to the determination of benzoylurea insecticides residues.