Community Reference Laboratories for Residues of Pesticides

Single Residue Methods

V a ria t ion of 1 ) QuEChERS-M e t hod

for V e ge t a ble Oil Sa m ple s
(fa t t y m a t rix w it hout w a t er)

1) Transfer 2 g of the homogenous sample into a

50 ml centrifuge tube.

2) Add 10 ml of acetonitrile, close the tube and shake vigorously

for 1 min.

3) Centrifuge for ~3 min at ~3000 rpm.

4) Transfer an aliquot (6 ml) of the acetonitrile phase (upper layer) into a 20 ml screw
capped vial.

5) Add ISTD-solution (10 µl /ml extract). Close the vial and shake for a few seconds.

Optionally transfer an aliquot of this raw extract into an auto-sampler vial and employ for the analysis of
pesticides with acidic groups.

6) Place the vial containing the extract for at least 1.5 hr in the freezer*.
* The removal of the residual lipids can also be achieved with the help of a silica-based reversed-phase
sorbent (ODS-, C18-type) as follows: Place 100 mg PSA and 100 mg ODS (25 mg of each per ml ex-
tract) in a 15 mL screw capped centrifuge tube and add 4 mL raw extract from 5). Continue with point
8). The freezing step can be skipped in this case.

7) Immediately separate the frozen co-extractives (frozen lipids) by filtration** through a

clean cotton wool into a 15 ml screw capped centrifuge tube containing
PSA (25 mg /ml extract).
** Instead of filtering, it is also possible to just centrifuge and/or decant the extract. In this case, take
care to avoid particles being carried over.

8) Close the tube, shake vigorously for 30 sec and centrifuge (for ~3 min at ~3000 rpm).

9) Transfer an aliquot of the cleaned-up extract into a screw capped storage vial.

10) Acidify slightly by adding formic acid solution 5% in acetonitrile (10 µl /ml extract).

11) Transfer the extract into auto-sampler vials to be used for gas- and liquid chroma-
tographic analysis.

Note: Highly non-polar pesticides (e.g. HCB, DDT) will have recoveries lower than 70%. The
recoveries are highly consistent however, so recovery correction using a factor is possible.
1)
Please see www.QuEChERS.com

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2) add 10ml acetonitrile
5) take aliquot

4) centrifuge
3) shake ~1min
3min/~3 00 0rpm

6) add ISTD solution

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12) adjust pH with 10µL/mL

HCOOH (5% in Acetonitrile)

9) 30sec D-SPE with

25mg /mL C18+PSA
+ 150mg/mL MgSO4

10) centrifuge 3min/~3 00 0rpm

11) take aliquot

Notes:
3 Highly lipophilic pesticides give recoveries <70% (e.g. DDT, HCB). The partitioning system and thus also the recoveries
achieved are, however, highly reproducible thus allowing the use of recovery correction factors.
3 The ISTD is added to an aliquot of the raw extract (after partitioning) to avoid result overestimations of the pesticides due
to ISTD-partitioning-losses.
3 Freezing-out of the raw extract has a similar lipid removal effect as D-SPE with ODS in