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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。
A method for the simultaneous determination of seven benzoylurea pesticide residues in water by UPLC-MS / MS / MS / MS / MS was established. After the sample was filtered and purified by HLB SPE, the target compound was eluted with 10 mL of dichloromethane and concentrated. After the volume of 1 mL of methanol was fixed, a BEH C18 column was used and water (5 mmol / L ammonium acetate) - acetonitrile as the mobile phase gradient elution, using tandem mass spectrometry as a detector for detection. The linear range of the 7 benzoylurea insecticides was good (r = 0.999 1 ~ 0.999 5), the recovery was 71.8% ~ 114% and the relative standard deviation was 3.3% ~ 18.8%. The detection limits From 7.0 to 16.0 ng / L. The method is rapid, sensitive and suitable for the determination of residues of seven benzoylurea insecticides in water.