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Validation of an analytical method to determine the content of patulin in apple juice and fruit puree
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Validation of an analytical method to determine the content of patulin in apple juice and fruit puree

Report on the final trial : determination of patulin in apple juice and fruit puree by liquid-liquid extraction and solid phase extraction with liquid chromatography using ultraviolet absorption : collaborative study

Validation of an analytical method to determine the content of patulin in apple juice and fruit puree

Report on the final trial : determination of patulin in apple juice and fruit puree by liquid-liquid extraction and solid phase extraction with liquid chromatography using ultraviolet absorption : collaborative study

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An interlaboratory comparison was carried out 10 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 solid phase clean-up (method A), whilst the others 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 10 ng/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 column for clean-up and evaporated. The residue was then re-dissolved in 0.1 % acetic acid 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 278 nm. For method B, the patulin was extracted three times from the juice or the de-pectinated 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. The juice and puree samples, both spiked and naturally contaminated with patulin, were sent to 43 laboratories in 17 countries. Test portions of the samples were spiked at levels of 10 ng/g and 25 ng/g for patulin. Recoveries in apple juice ranged from 37 - 123 % with an average of 73 % for method A and from 47 - 124 % with an average of 88 % for method B. Whereas in fruit puree recoveries ranged from 60 - 87 % with an average of 70 % in for method A and from 37 207 % with an average of 110 % for method B. Based on results for spiked samples (blind pairs at two levels), as well as naturally contaminated samples (blind pairs at three levels), the relative standard deviation for repeatability (RSDr) in juice ranged from 8.0 - 14.3 % for method A and from 5.0 - 37.6 % for method B. For puree these values ranged from 3.5 - 7.5 % for method A and from 8.4 - 27.7 % for method B. The relative standard deviation for repeatability (RSDR) in juice ranged from 39.5 - 10 8 % for method A and from 18.2 - 46.9 % for method B. For puree these values ranged from 12.5 - 27.7 % for method A and from 16.2 - 57.1 % for method B. 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.
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Catalogue number LA-NA-21008-EN-C
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ISSN ISBN DOI Catalogue number LA-NA-21008-EN-C
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