RT info:eu-repo/semantics/article T1 A new multiresponse optimization approach in combination with a D-Optimal experimental design for the determination of biogenic amines in fish by HPLC-FLD A1 Herrero Gutiérrez, Ana A1 Sanllorente Méndez, Silvia A1 Reguera Alonso, Celia A1 Ortiz Fernández, Mª Cruz A1 Sarabia Peinador, Luis Antonio K1 Multiresponse optimization K1 D-optimal design K1 Biogenic amines K1 HPLC-FLD K1 Derivatization K1 Fish K1 Chemistry K1 Mathematics K1 Química K1 Matemáticas AB A new strategy to approach multiresponse optimization in conjunction to a D-optimal design forsimultaneously optimizing a large number of experimental factors is proposed. The procedure is appliedto the determination of biogenic amines (histamine, putrescine, cadaverine, tyramine, tryptamine, 2-phenylethylamine, spermine and spermidine) in swordfish by HPLC-FLD after extraction with an acidand subsequent derivatization with dansyl chloride. Firstly, the extraction from a solid matrix and thederivatization of the extract are optimized. Ten experimental factors involved in both stages are studied,seven of them at two levels and the remaining at three levels; the use of a D-optimal design leads tooptimize the ten experimental variables, significantly reducing by a factor of 67 the experimental effortneeded but guaranteeing the quality of the estimates. A model with 19 coefficients, which includes thosecorresponding to the main effects and two possible interactions, is fitted to the peak area of each amine.Then, the validated models are used to predict the response (peak area) of the 3456 experiments of thecomplete factorial design. The variability among peak areas ranges from 13.5 for 2-phenylethylamine to122.5 for spermine, which shows, to a certain extent, the high and different effect of the pretreatment onthe responses. Then the percentiles are calculated from the peak areas of each amine. As the experimentalconditions are in conflict, the optimal solution for the multiresponse optimization is chosen fromamong those which have all the responses greater than a certain percentile for all the amines. Thedeveloped procedure reaches decision limits down to 2.5 mg L 1 for cadaverine or 497 mg L 1 for histamine in solvent and 0.07 mg kg 1 and 14.81 mg kg 1 in fish (probability of false positive equal to0.05), respectively. PB Elsevier YR 2016 FD 2016-11 LK http://hdl.handle.net/10259/4357 UL http://hdl.handle.net/10259/4357 LA eng NO MINECO (CTQ2014-53157-R) and FEDER funds DS Repositorio Institucional de la Universidad de Burgos RD 04-dic-2024