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Chlorinated Pesticide Residues in Olive Oil on Rxi®-5Sil MS

Pesticide Residues in Food Analysis

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Time (min)

GC_FF01044

Column

Rxi®-5Sil MS 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623)

Sample

Olive 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.:

130 °C (hold 0.5 min) to 330 °C at 5 °C/min

Carrier Gas

He, constant flow

Flow Rate:

1 mL/min

Detector

MS

Mode:

SIM

Transfer Line

Temp.:

320 °C

Ionization Mode: EI

Notes

Extraction 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.

For peak list, visit

www.restek.com

and enter

GC_FF01044 in the search

Similar to: (5%-phenyl)-methylpolysiloxane

GC COLUMNS |

APPLICATION-SPECIFIC COLUMNS

Foods, Flavors, & Fragrances

Rxi®-5Sil MS Columns

(fused silica)

(low-polarity phase; Crossbond® 1,4-bis(dimethylsiloxy)phenylene dimethyl polysiloxane)

• Engineered to be a low-bleed GC-MS column.

• Excellent inertness for active compounds.

• General-purpose columns—ideal for GC-MS analysis of semivolatiles, polycyclic

aromatic compounds, chlorinated hydrocarbons, phthalates, phenols, amines,

organochlorine pesticides, organophosphorus pesticides, drugs, solvent impurities,

and hydrocarbons.

• Temperature range: -60 °C to 350 °C.

The Rxi®-5Sil MS stationary phase incorporates phenyl groups in the polymer back-

bone. This improves thermal stability, reduces bleed, and makes the phase less prone

to oxidation. Rxi®-5Sil MS columns are ideal for GC-MS applications requiring high

sensitivity, including use in ion trap systems.

Rxi®-5Sil MS Structure

95%

5%

CH

3

CH

3

Si

O

O

CH

3

CH

3

Si

CH

3

CH

3

Si

similar phases

DB-5ms, DB-5msUI, VF-5ms, ZB-5ms,

ZB-SemiVolatiles, Rtx-5Sil MS

15-Meter

30-Meter

60-Meter

ID

df

temp. limits

cat.#

price

cat.#

price

cat.#

price

0.25 mm0.10 µm -60 to 320/350 °C 13605

13608

0.25 µm -60 to 320/350 °C 13620

13623

13626

0.50 µm -60 to 320/350 °C 13635

13638

1.00 µm -60 to 320/350 °C 13650

13653

13697

0.32 mm0.25 µm -60 to 320/350 °C 13621

13624

0.50 µm -60 to 320/350 °C

13639

1.00 µm -60 to 320/350 °C

13654

0.53 mm1.50 µm -60 to 320/330 °C

13670

10-Meter

20-Meter

40-Meter

60-Meter

ID

df

temp. limits cat.#

price

cat.#

price

cat.#

price

cat.#

price

0.15 mm0.15 µm -60 to 320/350 °C 43815

43816

2.0 µm -60 to 320/350 °C

43817

0.18 mm0.10 µm -60 to 320/350 °C

43607

0.18 µm -60 to 320/350 °C

43602

43605

0.36 µm -60 to 320/350 °C

43604

also

available

Comprehensive

203-compound

GC multiresidue

pesticide kit

See

page 568.