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Chlorinated Pesticide Residues in Olive Oil Rtx-CLPesticides2

GC_FF01043
PeaksQuant. ionQual. ion 1Qual. ion 2
1.α-BHC*219181109
2.γ-BHC219181109
3.β-BHC219181109
4.δ-BHC219181109
5.Heptachlor272237100
6.Aldrin263293220
7.Heptachlor epoxide26323781
8.δ-Chlordane27223765
9.α-Chlordane27223765
10.Endosulfan I195207241
PeaksQuant. ionQual. ion 1Qual. ion 2
11.4,4'-DDE246318176
12.Dieldrin79263277
13.Endrin26328181
14.4,4'-DDD235165199
15.Endosulfan II195207-
16.4,4'-DDT235165199
17.Endrin aldehyde67250345
18.Endosulfan sulfate272229239
19.Methoxychlor227274-
20.Endrin ketone67317281
* α-BHC not detected due to low recovery during sample preparation.
ColumnRtx-CLPesticides2, 30 m, 0.25 mm ID, 0.20 µm (cat.# 11323)
Standard/SampleOlive oil spiked with Organochlorine Pesticide Mix AB # 3 (cat.# 32415)
Conc.:10 µg/mL
Injection
Inj. Vol.:1 µL splitless (hold 0.5 min)
Liner:Single Taper w/Wool (cat.# 22286-200.1)
Inj. Temp.:225 °C
Oven
Oven Temp.:140 °C (hold 0.5 min) to 268 °C at 20 °C/min to 290 °C at 3 °C/min to 330 °C at 20 °C/min (hold 5 min)
Carrier GasHe, constant flow
Flow Rate:1 mL/min
DetectorMS
Mode:SIM
Transfer Line Temp.:320 °C
Ionization Mode:EI
NotesExtraction and dSPE Cleanup for Pesticide Residues in Olive Oil

Test sample: A 1.5 mL sample of commercially obtained virgin olive oil was spiked with a standard organochlorine pesticide mix. The spiked sample was processed as follows:
1. Dilute with 1.5 mL hexane.
2. Add 6 mL of acetonitrile (ACN).
3. Mix for 30 minutes on a shaker.
4. Allow layers to separate (approximately 20 minutes), then collect the top (ACN) layer.
5. Repeat the liquid-liquid extraction (steps 2–4) and combine both ACN extract layers.
6. Place 1 mL of the combined ACN extract in a 1.5 mL tube containing 150 mg magnesium sulfate and 50 mg PSA.
7. Shake the tube for 2 minutes.
8. Centrifuge at 3,000 U/min for approximately 5 minutes.
9. Remove the top layer and inject directly into the gas chromatograph system.