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C04021: Simultaneous determination of nivalenol and deoxynivalenol in maize and maize products using LC/MS/MS

Tuesday 15 August 2006

This research project aims to develop a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method of analysis for the mycotoxins nivalenol and deoxynivalenol in maize and a range of maize-based products, and to compare the results obtained with a traditional method.

Study Duration : September 2001 till December 2002

Contractor : LGC Ltd.

Background

The assessment of the two methods will enable the analyst, and ultimately the customer, to gain a much higher level of confidence in the results that are being produced for the analysis of nivalenol and deoxynivalenol in maize and maize products.

Research Approach

Seven replicate test portions of sample maize matrices were analysed after spiking at 20&#181g/kg (the required limit of quantification) with each compound, and a further seven test portions were analysed after spiking at 200&#181g/kg (ten times the required limit of quantification) with each compound.

Results and findings

The aim of this work was to develop a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method of analysis for the mycotoxins nivalenol and deoxynivalenol in maize and a range of maize based products, and to compare the results obtained with a traditional method.

Seven replicate test portions of sample maize matrices were analysed after spiking at 20&#181g/kg (the required limit of quantification) with each compound, and a further seven test portions were analysed after spiking at 200&#181g/kg (ten times the required limit of quantification) with each compound. In the case of popcorn, problems were encountered with the LC/MS/MS procedure, primarily related to the naturally incurred low levels of deoxynivalenol concentration in popcorn which made it impossible to quantify the recoveries of spiked material at the limit of quantification.

In the case of the traditional methods, three measurements were made after spiking with each compound, one at each of 250&#181g/kg, 500&#181g/kg and 1000&#181g/kg. A formal ruggedness test was undertaken on the LC/MS/MS procedure under repeatability conditions.

The outcomes of these tests comparing LC/MS/MS with high performance liquid chromotography (HPLC) with ultra-violet (UV) detection show that the results obtained using LC/MS/MS compare very favourably with those that have been obtained using a traditional method. The additional benefits of a superior limit of detection and the associated level of confidence in the peak identity is unsurpassed and thus give the analyst, and ultimately the customer, a much higher level of confidence in the results that are being produced.

Details of the LC/MS/MS method used are provided in the final report.

Dissemination information

The final report is available from the Agency's Information Centre.

To obtain a copy, please contact the Enquiry Desk, Information Services, Food Standards Agency (tel: 020 7276 8181/8182 or email: infocentre@foodstandards.gsi.gov.uk )

Contact : For any enquiries concerning this research project, please contact the relevant programme contact or email: science@foodstandards.gsi.gov.uk

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