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Develop a fully validated method for the determination of tartaric acid and tartrates in food based on the method previously developed by Agency funded research

Project Code: A01055

25/05/2007

LGC
Stuart, B ; Lawrance, P

Tartaric acid and it’s sodium, potassium or calcium salts are generally permitted additives for use in foodstuffs. To meet EU requirements for monitoring of food additives, robust, validated methods are needed for those foods in which the use of tartrates is permitted by the regulations. Methods are available for the determination of tartrates in wine and some foodstuffs but development and validation of methods was required to extend the scope to other foods.

Potential methods were evaluated in a previous project (FSA A1035) and a procedure for the determination of tartrate(s) in a range of foods was developed and successfully validated according to single laboratory validation principles. However tartrate recovery in two cooked samples was slightly low and the results from a second laboratory used to confirm method transferability were too variable.

The aim of this project was to complete the validation of the developed procedure to improve the robustness of the procedure if required. The method was then transferred to a second laboratory with supervision to investigate areas where problems could occur before conducting a mini-ring trial between the two laboratories with independent evaluation by a third, public analyst’s laboratory.

The method was optimised within LGC to improve the performance using a range of samples and was then further validated in-house, using a Plackett-Burmann robustness design. The SOP was then modified to reflect the findings of the investigation and robustness testing.

The modified method was then transferred to a second laboratory in a iterative manner so that problems in performing the procedure could be identified and addressed. This stage of the project demonstrated that the procedure could be sucessfully transferred to another laboratory providing that sufficient attention was given to following the procedure and optimising the HPLC conditions used. Some difficulties were experienced, particularly with fatty samples and the SOP was modified further, to accommodate this sample type.

The final SOP was then tested in a mini ring-trial between three laboratories, to compare method performance between experienced laboratories and a third, independent laboratory with no previous knowledge of the procedure. The third laboratory was a Public Analyst laboratory and therefore had considerable experience of HPLC methods in general but had not previously tried the SOP under test.

The results for all but one of the sample types , showed good agreement between the laboratories both in terms of accuracy and precision. The exception was for cocoa powder, where good agreement was obtained between laboratories 1 & 3, but laboratory 2 showed a very poor recovery (~ 34%). The reason for this is unclear but losses during sample clean-up are most likely.

In general, the final SOP gave good results for most sample types and it’s performance was demonstrated in three laboratories. It is therefore suitable for use in monitoring tartrate content of foods to support legislative requirements.

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