GC Analysis of Agriculture Pesticides in Orange (Spiked) on SLB®-5ms after QuEChERS Cleanup using Primary-Secondary Amine (PSA)

GC Analysis of Agriculture Pesticides in Orange (Spiked) on SLB®-5ms after QuEChERS Cleanup using Primary-Secondary Amine (PSA)


sample preparation SPE (Solid Phase Extraction)
sample/matrix 15 g of ground-up orange, 75 µL of the internal standard stock solution (ethoprophos at 20 ppm in methanol), 75 µL of the pesticide stock solution (29 pesticides, each at 20 ppm in methanol)
column SLB-5ms, 30 m x 0.25 mm I.D, 0.25 µm (28471-U)
oven 100 °C (1 min), 10 °C/min to 300 °C (5 min)
carrier gas helium, 1 mL/min constant
sample extract of an orange spiked with a 29-component pesticide mix plus 1 internal standard, each at 100 ppb
injection 1.0 µLpulsed (20 psi until 0.20 min), splitless (1.0 min)
liner 4 mm I.D., single taper
inj. temp. 250 °C
MSD interface 300 °C
scan range selected ion monitoring (SIM), 7 monitoring groups used


Analysis Note Chromatograms of the spiked orange samples are presented in the Figure. Several background peaks eluting prior to nine minutes are due to impurities in the toluene. Despite extract cleanup, matrix peaks are also present in the chromatograms. Further sample cleanup may be possible by increasing SPE sorbent weight. Nevertheless, all pesticides were detected. A first order fit was used for calibration. Linearity for the five-point calibration curves was excellent, with 28 of the 29 pesticides having r2 values >0.995 at a range of 50-500 ppb. Proper calibration of imazalil was not possible due to its presence in the orange blanks.
Categories Analytical Chromatography, SPE Applications, GC Applications, Pesticides, Herbicides
Featured Industry Agriculture
Food and Beverages
Legal Information SLB is a registered trademark of Sigma-Aldrich Co. LLC
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suitability application for GC, application for SPE


  • 4,4′-DDE (1,1-Dichloro-2,2-bis(p-chlorophenyl)ethylene)
  • Acephate
  • Captan
  • Carbaryl
  • Chlorothalonil
  • Chlorpyrifos
  • cis-Chlordane
  • cis-Permethrin
  • Coumaphos
  • Cyprodinil
  • Diazinon
  • Dichlofluanid
  • Dichlorvos
  • Dicofol
  • Dieldrin
  • Endosulfan sulfate
  • Ethoprophos
  • Folpet
  • Hexachlorobenzene
  • Imazalil
  • Lindane
  • Methamidophos
  • Methyl chloropyrifos
  • p-Dichlorobenzophenone
  • Penconazole
  • Propoxur
  • Thiabendazole
  • Tolylfluanid
  • trans-Permethrin
  • γ-BHC


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