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

Determination of Carbamates in Soil and Sediment Using UPLC-MS/MS

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%.