摘要
利用超高效液相色谱-串联质谱,建立土壤和沉积物中痕量氨基甲酸酯农药的分析方法。该方法用体积比1∶1的二氯甲烷/甲醇对土壤和沉积物样品进行加速溶剂萃取,GCB/PSA固相萃取小柱对萃取液进行净化,内标法定量,用超高效液相色谱-串联质谱法分析土壤和沉积物中20种氨基甲酸酯农药。20种氨基甲酸酯农药在0.02~1.0μg/mL范围内线性良好(r≥0.99),检测限为0.20~0.60 ng/g。沉积物加标样品(20ng/g)和土壤加标样品(20ng/g)的回收率分别为33.2%~101.9%、38.8%~120.5%,相对标准偏差为6.1%~28.0%、2.3%~16.0%。沉积物加标样品(2.0 ng/g)回收率为43.0%~100.0%,相对标准偏差为2.1%~11.3%。
An analytical method,using Solid Phase Extraction and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),was determined for carbamates in soil and sediment.Accelarate solvent extraction(ASE) was used to performe extraction with V/V=1∶1 dichlormethanol and methanol,and the sample was then cleaned by GCB/PSA extaction column.UPLC-MS/MS was used to quantification with internal standard.It was shown that,the method presented good linear correlation between 0.002-0.1 μg/mL,with coefficient factor being larger than 0.99.At the same time,the detection limits were in range of 0.20-0.60 ng/g.The recoveries of spiked sediment sample(20 ng/g) and spiked soil sample(20 ng/g) were 33.2%-101.9%,38.8%-120.5%,respectively with the RSD were 6.1%-28.0%,2.3%-16.0%.The recoveries of spiked sediment sample(2.0 ng/g) was 43.0%-100.0% and the RSD was 2.1%-11.3%.
出处
《中国环境监测》
CAS
CSCD
北大核心
2013年第4期103-106,共4页
Environmental Monitoring in China
基金
国家标准制定项目(2009-1055)
浙江省环保科技项目(200805
200927
2010A06)