摘要
采用气相色谱-串联质谱(GC-MS/MS)对毒鱼事件中水、鱼肉和饲料中的10种拟出虫菊酯农药定量检测。水样用三氯甲烷液液萃取,鱼肉和饲料用快速溶剂萃取仪(ASE)萃取后,再经C18固相萃取柱净化,冷冻离心机离心后取上清液,用气相色谱-串联质谱检测,采用正离子扫描多反应监测模式对农药进行定性定量分析。结果表明:10种农药在0.01～0.50μg/mL质量浓度范围内具有良好的线性关系,相关系数为(r2)不小于0.980 5;在水、鱼肉和饲料中,3个浓度添加水平下农药的回收率为81.2～113.8%,精密度(RSD,n=6)为1.5～6.9%;检出限(LOD)为0.06～2.89μg/L,定量限(LOQ)为0.25～11.55μg/L。试验结果表明该方法简单、快速、准确有效,可用作对毒鱼事件中水、鱼肉和饲料中菊酯类农药的测定。
Ten pyrethroid pesticides in the water, fish and bait of the tainted-fish events were analyzed by gas chromatography-tandem mass spectrometry （GC-MS/MS） in the present work. The water samples were ex- tracted with chloroform, fish and bait samples were extracted by Accelerated Solvent Extraction （ASE） meth- od. All the samples were cleaned by C18 solid phase extraction （SPE）, and carried out qualitative and quan- titative test using GC-MS/MS. The result showed that 10 pesticides showed a good linear relationship at the concentration of 0. 0143.50 ug/mL, with the correlation coefficient R2 higher than 0. 980 5. The average re- coveries of different addition levels in the water, fish and bait were 81.2% -113.8% , the relative standard deviations （RSD, n = 6） were 1.5%-6.9% , detection limits （LOD） were 0.06-2.89 μg/L, and limits of quantification （LOQ） were 0.25-11.55 μg/L. It＇s justified that the tested method is simple, quick, accurate and effective, and may be used to detect the residues of pyrethroid pesticides in the water, fish and bait.
出处
《山地农业生物学报》
2012年第6期538-543,共6页
Journal of Mountain Agriculture and Biology
关键词
菊酯类农药
固相萃取
气相色谱-串联质谱
Pyrethroids pesticide
Solid-phase extraction
Gas chromatography-tandem mass spectrometry
