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86
www.restek.comChlorinated 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.comand 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.