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Extraction of Organochlorine Pesticides in Animal Feed

Relevant for: Food Industry, Environmental, Chemical Industry

Contaminations of animal feed by polychlorinated pesticides, like Lindane (γ-HCH) and its
congeners, or DDT, are a considerable risk to human beings. Although the use of the
polychlorinated pesticides was banned for several years, they are still frequently detected in fat
containing material owing to their persistence, toxicology, lipophilic properties and
bioaccumulation.

Figure 1: Multiwave PRO Extraction


1 Introduction

3 Experimental
In order to accurately determine the accumulated
polychlorinated compounds an efficient microwave-
assisted extraction method was developed. 3.1 Sample

 BCR 115 – animal feed (2 g)


2 Instrumentation

3.2 Extraction solvent


The extractions were performed with the microwave
reaction system Multiwave 3000 (with Rotor 8SOLV 30 mL n-Hexane - Acetone 1:1 (v/v)
and magnetic stirring device) by Anton Paar, which is
the predecessor of Multiwave PRO SOLV.
Using Rotor 16SOLV MF100 and the p/T-sensor the
method is reliably adaptable to Multiwave PRO SOLV.
The determination of the investigated organochlorine
pesticides was carried out by GC-MS (Hewlett-
Packard, HP6890 and HP5973) in SIM-Mode.
Figure 1: Extraction Program in Multiwave PRO SOLV
Calibration was accomplished by internal
standardization with isotope labeled standards.

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4 Results

As it can be seen from the results (table 1), the data


are in good agreement with the certified value.

Compound Certified Value Found Value


(ng g-1) (ng g-1)
Hexachlorobenzene 19.4 ± 1.4 20.0 ± 0.1
β-HCH 23 ± 3 25.2 ± 0.2
γ-HCH 21.8 ± 2.0 25.3 ± 0.6
Heptachlor 19.0 ± 1.5 18.2 ± 0.2
γ-Chlordane 48 ± 13 50.8 ± 1.4
α-Endosulfan 46 ± 4 47.3 ± 0.5
Dieldrin 18 ± 3 20.1 ± 0.4
Endrin 46 ± 6 48.6 ± 0.2
p,p’-DDE 47 ± 4 49.0 ± 0.2
o,p’-DDT 46 ± 5 45.2 ± 0.3
Table 1: Recovery from BCR 115 (n=4)

5 Conclusion

By using stirred closed vessels, extraction of 16


samples in parallel can be done within 40 min. Fast
extraction, better control, complete documentation as
well as reduced solvent amounts are offered by MAE
in Multiwave PRO SOLV. The good recoveries with
only small variations deviations indicates the precision
of the method.

6 References

Marion Gfrerer, Ernst Lankmayr


Institute for Analytical Chemistry, Micro- and
Radiochemistry, Graz University of Technology

Contact Anton Paar GmbH


Tel: +43 316 257-0
asc@anton-paar.com | www.anton-paar.com

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