超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药

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0.02～1.0 μg/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(20rg/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％.