A multivariate optimization process of the sample extraction procedure by Box-Behnken design through a global desirability function is described for the determination of six non-dioxin-like polychlorinated biphenyls(N...A multivariate optimization process of the sample extraction procedure by Box-Behnken design through a global desirability function is described for the determination of six non-dioxin-like polychlorinated biphenyls(NDL-PCBs#28,52,101,153,138 and 180)in milk by GC-ECD and mass spectrometry.Three factors were involved in refining the extraction conditions:the acetone percentage in the extraction mixture,the sample/solvent ratio,and the extraction time.The three-factor design required 26 experiments that were carried out in duplicate and in a randomized order to minimize the bias effects of uncontrolled variables.The optimized factors(acetone percentage:30%;sample-to-solvent ratio:0.11 g mL^-1;extraction time:45 min)ensured a low solvent consumption and a reduced extraction time,allowing a rapid and simultaneous preparation of multiple sample extracts.The method was validated according to the European directives(Decision 657/2002/EC,SANTE 2017/11813/EC)through the evaluation of linearity,selectivity,LOD,LOQ,recovery,precision,and ruggedness.展开更多
文摘A multivariate optimization process of the sample extraction procedure by Box-Behnken design through a global desirability function is described for the determination of six non-dioxin-like polychlorinated biphenyls(NDL-PCBs#28,52,101,153,138 and 180)in milk by GC-ECD and mass spectrometry.Three factors were involved in refining the extraction conditions:the acetone percentage in the extraction mixture,the sample/solvent ratio,and the extraction time.The three-factor design required 26 experiments that were carried out in duplicate and in a randomized order to minimize the bias effects of uncontrolled variables.The optimized factors(acetone percentage:30%;sample-to-solvent ratio:0.11 g mL^-1;extraction time:45 min)ensured a low solvent consumption and a reduced extraction time,allowing a rapid and simultaneous preparation of multiple sample extracts.The method was validated according to the European directives(Decision 657/2002/EC,SANTE 2017/11813/EC)through the evaluation of linearity,selectivity,LOD,LOQ,recovery,precision,and ruggedness.
