建立了西瓜样品中喹啉铜农药残留的超高效液相色谱分析方法.样品用4%冰醋酸超声振荡提取,提取液经阳离子交换固相萃取小柱净化后,用1%醋酸铵-甲醇洗脱,洗脱液经氮气吹干后用流动相定容.试样采用Vneusil MP C18色谱柱(150 mm ×4.6 mm,5μm)进行分离,流动相为0.1%三氟乙酸-乙腈(95>5).结果表明,喹啉铜在0.05~10 μg/mL浓度范围内线性关系良好,相关系数不低于0.999 9.在0.05~2.0 mg/kg加标浓度范围内的平均回收率为72.3% ~84.1%,相对标准偏差为2.1%~3.8%,方法的检出限为0.024 mg/kg.
A novel method for the determination of copper 8-quinolinolate by ultra-performance liquid chromatography(UPLC) was developed.The sample was extracted with 4% acetic acid solution and cleaned up with a Cleanert PCX cartridge.The cartridge was eluted with 1% ammonium acetate-methanol.The elution was evaporated to near dryness under a stream of nitrogen,and dissolved by mobile phase.The target compound was separated on a Vneusil MP C18 column(150 mm ×4.6 mm,5 μm) using 0.1% TFA-acetonitrile (95 ∶ 5) as mobile phase.The method had a good linear correlation(r≥0.999 9)in the range of 0.05-10 μg/mL.The average recoveries of copper 8-quinolinolate at a spiked range of 0.05-2.0 mg/kg were in the range of 72.3%-84.1% with relative standard deviations(RSDs) of 2.1%-3.8%.The limit of detection(LOD) was 0.024 mg/kg.