Box Behnken design-based optimized extraction of non-dioxin-like PCBs for GC-ECD and GC-MS analyses in milk samples  

作　　者：Valeria Nardelli Valeria D’Amico Ines Della Rovere Francesco Casamassima Wadir Mario Valentino Marchesiello Donatella Nardiello Maurizio Quinto 

机构地区：[1]Istituto Zooprofilattico Sperimentale della Puglia e della Basilicata,Via Manfredonia 20,Foggia,71121,Italy [2]Dipartimento di Scienze Agrarie,degli Alimenti e dell’Ambiente-Universita degli Studi di Foggia,Via Napoli,25,71122,Foggia,Italy [3]Key Laboratory of Natural Resources of the Changbai Mountain and Functional Molecules,Yanbian University,Park Road 977,133002,Yanji,China

出　　处：《Emerging Contaminants》2020年第1期303-311,共9页新兴污染物（英文）

摘　　要：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.

关 键 词：NDL-PCBs Box behnken experimental design MILK GC-ECD Extraction process optimization Method validation 

分 类 号：O62[理学—有机化学]