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Figure 1 Chlorinated pesticide residues in olive oil are easily
separated on either Rtx®-CLPesticides2 or Rxi®-5Sil MS columns.
• 13 • 2008 vol. 3
A. Rtx®-CLPesticides2
Qual. Qual.
Compound Quant. ion ion 1 ion 2
*1. α-BHC 219 181 109
2. γ-BHC 219 181 109
3. β-BHC 219 181 109
4. δ-BHC 219 181 109
5. heptachlor 272 237 100
6. aldrin 263 293 220
7. heptachlor epoxide 263 237 81
8. δ-chlordane 272 237 65
9. α-chlordane 272 237 65
10. endosulfan I 195 207 241
11. 4,4'-DDE 246 318 176
12. dieldrin 79 263 277
13. endrin 263 281 81
14. 4,4'-DDD 235 165 199
15. endosulfan II 195 207 -
16. 4,4'-DDT 235 165 199
17. endrin aldehyde 67 250 345
18. endosulfan sulfate 272 229 239
19. methoxychlor 227 274 -
20. endrin ketone 67 317 281
* not present
Column: A. Rtx®-CLPesticides2, 30m,
0.25mm ID, 0.20µm (cat.# 11323)
B. Rxi®-5Sil MS, 30m, 0.25mm ID,
0.25µm (cat.# 13623)
Sample: 10µg/mL Organochlorine Pesticide
Mix AB # 3 (cat.# 32415)
in olive oil
Inj.: 1µL, splitless (hold 0.5 min.),
3.5mm single gooseneck liner
(cat.# 20962) packed with wool
Inj. temp.: 225°C
Carrier gas: helium, constant flow
Flow rate: 1mL/min.
Oven temp.: A. 140°C (hold 0.5 min.) to 268°C @
20°C/min. to 290°C @ 3°C/min.
to 330°C (hold 5 min.) @ 20°C/min.
B. 130°C (hold 0.5 min.) to 330°C
@ 5°C/min
Det: MS
Transfer line temp.: 320°C
Ionization: EI
Mode: SIM
GC_FF01043
B. Rxi®-5Sil MS
GC_FF01044
Product Listing
dSPE Tube for Clean-Up of Pesticide
Residue Samples
PSA—primary and secondary amine exchange material.
Description Material Methods qty. cat# price
Resprep
Q250
150mg MgSO4 ,
50mg PSA
AOAC
2007.1 100-pk. 26124
2mL Microentrifuge Tubes for dSPE
aldrin
α-BHC
β-BHC
δ-BHC
γ-BHC (lindane)
α-chlordane
γ-chlordane
4,4'-DDD
4,4'-DDE
4,4'-DDT
dieldrin
endosulfan I
endosulfan II
endosulfan sulfate
endrin
endrin aldehyde
endrin ketone
heptachlor
heptachlor epoxide (isomer B)
methoxychlor
Organochlorine Pesticide Mix AB # 3
(20 components)
2,000µg/mL each in hexane:toluene (1:1), 1mL/ampul
cat. # 32415 (ea.)
Rtx®-CLPesticides2 Columns (fused silica)
ID df (µm) temp. limits length cat. # price
0.25mm 0.20 -60 to 320/340°C 30-Meter 11323
Rxi®-5Sil MS Columns (fused silica)
(Crossbond®, selectivity close to 5% diphenyl/95% dimethyl
polysiloxane)
ID df (µm) temp. limits length cat. # price
0.25mm 0.25 -60 to 330/350°C 30-Meter 13623
spectrometer detector (MSD). Only α-BHC was
not detected, a subject of further investigation,
however either column can be used effectively.
Recoveries of 70%-80%were obtained, levels com-
parable to conventional SPE—without the necessity
of vacuum manifolds or high pressure systems.
The GPC method attained recoveries of > 95%.
However this method requires large amounts of sol-
vent and takes over twice as long as other methods.
The dSPE method shown here is an efficient, cost-
effective way to clean up chlorinated pesticide
residues in olive oil. With good recoveries and
minimal matrix interference, it is an easy way to
reduce solvent usage, compared to conventional
SPE, and is more cost-effective than GPC.
References
1. C. Lentza-Rizos, E.J. Avramides, Rev. Environ. Contam. Toxicol. 141
(1995) 111.
2. S. Cunha, S. Lehotay, K. Mastovska, J. Sep. Sci. 30 (2007) 620.
3. M. Crawford, M. Halvorson, J. Stevens, The Examination and
Automation of GPC, SPE and QuEChERS Utilized in Extracting
Pesticides from Olive Oil. HPLC 2008 poster presentation.
800-356-1688 •