Optimization of a FIA system with amperometric detection by means of a desirability function Determination of sulfadiazine, sulfamethazine and sulfamerazine in milk

A sensitive and cheap FIA, with amperometric detection, analytical procedure is developed in this paper to determine sulfadiazine, sulfamethazine and sulfamerazine in milk. A multicriteria optimization based on the use of a desirability function is used for optimizing two analytical responses (peak...

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Bibliographic Details
Published in:Talanta (Oxford) 2008-03, Vol.75 (1), p.274-283
Main Authors: REGUERA, Celia, CRUZ ORTIZ, M, HERRERO, Ana, SARABIA, Luis A
Format: Article
Language:English
Subjects:
Analytical chemistry
Animals
Cattle
Chemistry
Electric Conductivity
Electrochemical methods
Exact sciences and technology
Fluoroimmunoassay - economics
Fluoroimmunoassay - methods
Milk - chemistry
Sulfadiazine - analysis
Sulfamerazine - analysis
Sulfamethazine - analysis
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Summary:A sensitive and cheap FIA, with amperometric detection, analytical procedure is developed in this paper to determine sulfadiazine, sulfamethazine and sulfamerazine in milk. A multicriteria optimization based on the use of a desirability function is used for optimizing two analytical responses (peak height and its variability) since single-objective optimizations lead to conflicting experimental conditions. In the optimum conditions, the determination of the three sulfonamides in milk samples is carried out, the analytical procedure being validated according to Commission Decision 2002/657/EC. The decision limit at 0 and 100 microg L(-1) (which is the maximum residue limit in milk) are 13.9 and 110.2, 9.5 and 107.1 and 9.1 and 107.1 microg L(-1) for sulfadiazine, sulfamethazine and sulfamerazine, respectively. Whereas the values of capability of detection, CCbeta, obtained at 0 and 100 microg L(-1) were 26.9 and 119.8, 18.2 and 113.6, and 17.5 and 113.7 microg L(-1) for sulfadiazine, sulfamethazine and sulfamerazine, respectively. Recovery values between 67.4% and 119.1% are found for milk test samples of two brands of milk. The accuracy of the method is confirmed. The ruggedness of the procedure is evaluated by means of a Plackett-Burman design. The relative errors were lower than 2.5% (n=7).
ISSN:0039-9140
1873-3573
DOI:10.1016/j.talanta.2007.11.030