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采用高效液相色谱-串联质谱法对土壤中的农药进行多残留分析。

Multiresidue analysis of pesticides in soil by high-performance liquid chromatography with tandem mass spectrometry.

作者信息

Fenoll José, Hellín Pilar, Martínez Carmen M, Flores Pilar

机构信息

Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario, IMIDA, C/Mayor s/n, La Alberca 30150 Murcia, Spain.

出版信息

J AOAC Int. 2009 Sep-Oct;92(5):1566-75.

Abstract

An analytical multiresidue method using HPLC/MS/MS with a triple-quadrupole mass spectrometer in the multiple reaction monitoring mode for the simultaneous determination of 54 pesticides in soil has been developed. The procedure involved initial single-phase extraction of soil sample with acetonitrile by sonication, followed by liquid-liquid partitioning after addition of NaCI. The average recovery by the HPLC/MS/MS method obtained for these compounds varied from 63.2 to 113.8%, with an RSD between 1.9 and 7.1%. The method gave good linearity over the assay range of 10-500 microg/L (except famoxadone, 50-1000 microg/L); the LOD and LOQ for the pesticides varied from 0.02 to 13.2 and from 0.1 to 43.9 microg/kg, respectively. The proposed method was used to determine pesticide levels in soil samples from two experimental vineyards and two tomato greenhouses.

摘要

已开发出一种采用高效液相色谱/串联质谱联用仪(HPLC/MS/MS)和三重四极杆质谱仪,在多反应监测模式下同时测定土壤中54种农药的分析多残留方法。该方法包括先用乙腈对土壤样品进行超声单阶段萃取,然后加入氯化钠进行液液分配。通过HPLC/MS/MS方法获得的这些化合物的平均回收率在63.2%至113.8%之间,相对标准偏差在1.9%至7.1%之间。该方法在10 - 500微克/升的测定范围内具有良好的线性(恶唑菌酮除外,为50 - 1000微克/升);这些农药的检测限和定量限分别在0.02至13.2微克/千克和0.1至43.9微克/千克之间。所提出的方法用于测定来自两个实验葡萄园和两个番茄温室的土壤样品中的农药含量。

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