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Abstract

An interlaboratory comparison was carried out to evaluate the effectiveness of 2 different methods. One method was developed at the Joint Research Centre and is based on single forced liquid-liquid extraction with slid phase clean-up (method A), whilst the other is based on repetitive liquid-liquid extraction (method B). The latter method is a slightly modified version with the same principle as one that is currently discussed as a CEN standard. The main modifications were made in terms of aliquotation in this method. Both methods were tested for the determination of patulin in apple juice and fruit puree at the proposed European regulatory limit of 10ng/g. For method A, the test portion of the sample was extracted with ethylacetate-hexane (6+4[v+v]). The sample extract was centrifuged, passed over a silicagel colum for clean-up and evaporated. The residue was then re-dissolved in o.1% acetic solution. The separation and determination of the patulin was performed by reverse-phase high performance liquid chromatography (HPLC) and detected by ultraviolet (UV) absorption at 278nm.

For method B, the patulin was extracted three times from the juice or the depectinated puree with neat ethylacetate (EtAc). The combined EtAc phases were re-extracted with sodium carbonate solution and evaporated. The residue was then re-dissolved in 0.1% acetic acid solution and separated by HPLC as in method A.

Method A showed acceptable within-laboratory and between-laboratory precision for both matrices, while method B showed some limitation for fortified materials in puree concerning the required precision performance.

Additional information

Authors: ARRANZ I, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);STROKA J, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);KROEGER K, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);DERBYSHIRE M, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);MISCHKE C, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);ANKLAM E, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE)
Bibliographic Reference: EUR 21008 EN (2004), various paging. Free of charge
Availability: Available from European Commission, JRC Knowledge Management Unit, Ispra (IT) Tel: +39 033278 9893 Fax: +39 033278 5409 E-mail: jrc-publications-office@ec.europa.eu or Bruxelles (BE) Tel: +32 2 295 76 24 Fax: +32 2 299 63 22
Record Number: 200417531 / Last updated on: 2004-06-02
Category: PUBLICATION
Original language: en
Available languages: en