摘要
开发了一种在线固相萃取技术结合高效液相色谱-串联质谱法的新颖分析方法,旨在实现对水体中12种新烟碱类农药残留的高效、准确检测。水样经0.22μm针式滤头过滤后直接上机检测,在线富集后进入色谱柱分离,用乙腈和纯水作流动相梯度洗脱,采用多反应监测模式(MRM),用内标法定量分析。12种农药的线性关系表现优异,相关系数(R2)均大于0.997。其检出限范围在0.3~3.0 ng/L之间,加标回收率则在67.1%~112.7%区间内波动,而相对标准偏差(RSD)则控制在1.0%~4.8%。与常规的检测方法相比,此方法具有显著优势:检测时间大幅缩短、试剂用量显著减少、检出限明显降低以及分析效率显著提升。此检测法适用于水体中新烟碱类农药的检测。
A novel analytical method has been developed that combines online solid-phase extraction with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),aiming to achieve efficient and accurate detection of 12 neonicotinoid pesticide residues in water bodies.Water samples are filtered through a 0.22μm syringe filter and directly injected into the instrument for detection.Online enrichment is followed by separation on a chromatographic column,with acetonitrile and water used as the mobile phase for gradient elution.Multi-reaction monitoring(MRM)mode is employed,and quantitative analysis is conducted using the internal standard method.The linear relationships for the 12 pesticides exhibit excellent performance,with correlation coefficients(R~2)all greater than 0.997.The detection limits range from 0.3 to 3.0 ng/L,while the spiking recovery rates fluctuate between 67.1%and 112.7%.The relative standard deviations(RSD)are controlled within the range of 1.0%to 4.8%.Compared with conventional detection methods,this method offers significant advantages,including a substantial reduction in detection time,a notable decrease in reagent consumption,a marked lowering of detection limits,and a significant improvement in analytical efficiency.Therefore,making it suitable for the detection of neonicotinoid pesticides in water bodies.
作者
王金玲
WANG Jinling(Shenzhen Academy of Environmental Science,Shenzhen 518000,Guangdong,China)
出处
《四川化工》
2025年第1期23-27,共5页
Sichuan Chemical Industry
关键词
水
新烟碱类农药
在线固相萃取
高效液相色谱-串联质谱法
检测
water
neonicotinoid pesticides
online solid phase extraction
high performance liquid chromatography-tandem mass spectrometry
detection
