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G003590

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

suitable for GC, application for SPE

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About This Item

technique(s)

gas chromatography (GC): suitable
solid phase extraction (SPE): suitable

test parameters

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)
inj. temp.: 250 °C
MSD interface: 300 °C
scan range: selected ion monitoring (SIM), 7 monitoring groups used
carrier gas: helium, 1 mL/min constant
injection: 1.0 μL pulsed (20 psi until 0.20 min), splitless (1.0 min)
liner: 4 mm I.D., single taper
sample: extract of an orange spiked with a 29-component pesticide mix plus 1 internal standard, each at 100 ppb

suitability

application for SPE

application(s)

agriculture
food and beverages

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.

Legal Information

SLB is a registered trademark of Merck KGaA, Darmstadt, Germany

Analyte

Description
    Dichlorvos
    Acephate
    Propoxur
    Hexachlorobenzene
    Lindane
    Diazinon
    Chlorothalonil
    Carbaryl
    Dichlofluanid
    Chlorpyrifos
    Cyprodinil
    Tolylfluanid
    Captan
    Thiabendazole
    Folpet
    cis-Chlordane
    Imazalil
    4,4′-DDE
    Dieldrin
    Endosulfan sulfate
    Dicofol
    cis-Permethrin
    trans-Permethrin
    Coumaphos
    See All (24)

Analytical column

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