Graphene based solid phase extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry for carbamate pesticides analysis in environmental water samples

J Chromatogr A. 2014 Aug 15:1355:219-27. doi: 10.1016/j.chroma.2014.05.085. Epub 2014 Jun 12.

Abstract

In this paper, graphene, a new sorbent material, was synthesized and used for solid-phase extraction (SPE) of the six carbamate pesticides (pirimicarb, baygon, carbaryl, isoprocarb, baycarb and diethofencarb) in environmental water samples. The target analytes can be extracted on the graphene-packed SPE cartridge, and then eluted with acetone. The eluate was collected and dried by high purity nitrogen gas at room temperature. 1mL of 20% (v/v) acetonitrile aqueous solution was used to redissolve the residue. The final sample solution was analyzed by ultra performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) system. Under optimum conditions, good linearity was obtained for the carbamates with correlation coefficient in the range of 0.9992-0.9998. The limits of detection (S/N=3) for the six carbamate pesticides were in the range of 0.5-6.9ngL(-1). Relative standard deviations (RSD) for five replicate determinations were below 5.54%. RSD values for cartridge-to-cartridge precision (n=7) were in the range of 1.27-8.13%. After proper regeneration, the graphene-packed SPE cartridge could be re-used over 100 times for standard solution without significant loss of performance. The enrichment factors for the target analytes were in the range of 34.2-51.7. The established method has been successfully applied to the determination of carbamate pesticide residues in environmental water samples such as river water, well water and lake water.

Keywords: Carbamate pesticides; Environmental water; Graphene; SPE; UPLC–MS/MS.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbamates / analysis*
  • Chromatography, High Pressure Liquid / methods*
  • Fresh Water / analysis*
  • Graphite / chemistry*
  • Hydrogen-Ion Concentration
  • Microscopy, Electron, Scanning
  • Microscopy, Electron, Transmission
  • Pesticide Residues / analysis*
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods*
  • Water Pollutants, Chemical / analysis

Substances

  • Carbamates
  • Pesticide Residues
  • Water Pollutants, Chemical
  • Graphite