title: A new multiresponse optimization approach in combination with a D-Optimal experimental design for the determination of biogenic amines in fish by HPLC-FLD.
abstract: A new strategy to approach multiresponse optimization in conjunction to a D-optimal design for simultaneously optimizing a large number of experimental factors is proposed. The procedure is applied to the determination of biogenic amines (histamine, putrescine, cadaverine, tyramine, tryptamine, 2-phenylethylamine, spermine and spermidine) in swordfish by HPLC-FLD after extraction with an acid and subsequent derivatization with dansyl chloride. Firstly, the extraction from a solid matrix and the derivatization 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 to optimize the ten experimental variables, significantly reducing by a factor of 67 the experimental effort needed but guaranteeing the quality of the estimates. A model with 19 coefficients, which includes those corresponding 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 the complete factorial design. The variability among peak areas ranges from 13.5 for 2-phenylethylamine to 122.5 for spermine, which shows, to a certain extent, the high and different effect of the pretreatment on the responses. Then the percentiles are calculated from the peak areas of each amine. As the experimental conditions are in conflict, the optimal solution for the multiresponse optimization is chosen from among those which have all the responses greater than a certain percentile for all the amines. The developed procedure reaches decision limits down to 2.5 μg L-1for cadaverine or 497 μg L-1for histamine in solvent and 0.07 mg kg-1and 14.81 mg kg-1in fish (probability of false positive equal to 0.05), respectively.
authors.affiliation: Dept. of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Bañuelos s/n, 09001 Burgos, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Herrero
authors.affiliation: Dept. of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Bañuelos s/n, 09001 Burgos, Spain.
authors.forename: S
authors.initials: S
authors.lastname: Sanllorente
authors.affiliation: Dept. of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Bañuelos s/n, 09001 Burgos, Spain.
authors.forename: C
authors.initials: C
authors.lastname: Reguera
authors.affiliation: Dept. of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Bañuelos s/n, 09001 Burgos, Spain. Electronic address: mcortiz@ubu.es.
authors.forename: M C
authors.initials: MC
authors.lastname: Ortiz
authors.affiliation: Dept. of Mathematics and Computation, Faculty of Sciences, University of Burgos, Plaza Misael Bañuelos s/n, 09001 Burgos, Spain.
authors.forename: L A
authors.initials: LA
authors.lastname: Sarabia
mesh_terms: D000818:Animals; D001679:Biogenic Amines / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005399:Fishes; D057230:Limit of Detection; D012015:Reference Standards; D015203:Reproducibility of Results
chemical_list: D001679:Biogenic Amines
keywords: Biogenic amines; D-optimal design; Derivatization; Fish; HPLC-FLD; Multiresponse optimization