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

Propiedades

• 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

Descripción

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

Analito

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
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