PMID- 27178547 OWN - NLM STAT- MEDLINE DCOM- 20180117 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 408 IP - 18 DP - 2016 Jul TI - A validated method for rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in human milk: focus on utility of tandem solid phase extraction (SPE) cleanup. PG - 4897-906 LID - 10.1007/s00216-016-9576-y [doi] AB - An improved method based on tandem solid phase extraction (SPE) cleanup and gas chromatography-high resolution mass spectrometry (GC-HRMS) has been validated for a rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), dioxin-like polychlorinated biphenyls (PCBs), marker polychlorinated biphenyls (M-PCBs), and polybrominated diphenyl ethers (PBDEs) using a large volume (50 mL) of human milk. This method was well validated for the measurement of these analytes in human milk from the general population with low limits of detection (LODs, 0.004-0.12 ng/g lipid), satisfactory accuracy (75-120 % of recoveries), and precision [less than 10 % of relative standard deviations (RSDs)]. To comprehensively evaluate the performance of this method, a good, presently validated and routinely used method based on an automated sample clean-up system (ASCS, based on the commercial acid multilayer silica, basic alumina, and carbon columns) was used in parallel for comparison. Compared with the ASCS method, this method presented comparable specificity. Additionally, this method, in contrast to ASCS method, highly reduced consumption of solvents (40 mL versus 500 mL), which results in much lower background in the procedural blank, reduced time, and enhanced sample pretreatment throughput. This method was also applied in a pilot study to measure a batch of human milk samples with satisfactory results. Graphical Abstract Characteristics of the application of tandem SPE cleanup for determination of PCDD/Fs, DL-PCBs,M-PCBs and PBDEs in human milk. FAU - Lin, Yuanjie AU - Lin Y AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. FAU - Feng, Chao AU - Feng C AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. FAU - Xu, Qian AU - Xu Q AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. FAU - Lu, Dasheng AU - Lu D AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. ludasheng@scdc.sh.cn. AD - School of Public Health/MOE Key Lab for Public Health/Collaborative Innovation Center of Social Risks Governance in Health, Fudan University, 130 Dong'an Road, Shanghai, 200032, China. ludasheng@scdc.sh.cn. FAU - Qiu, Xinlei AU - Qiu X AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. FAU - Jin, Yu'e AU - Jin Y AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. FAU - Wang, Guoquan AU - Wang G AD - Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. wangguoquan@scdc.sh.cn. FAU - Wang, Dongli AU - Wang D AD - California Department of Public Health, 850 Marina Bay Parkway, Richmond, CA, 94804, USA. FAU - She, Jianwen AU - She J AD - California Department of Public Health, 850 Marina Bay Parkway, Richmond, CA, 94804, USA. FAU - Zhou, Zhijun AU - Zhou Z AD - School of Public Health/MOE Key Lab for Public Health/Collaborative Innovation Center of Social Risks Governance in Health, Fudan University, 130 Dong'an Road, Shanghai, 200032, China. LA - eng PT - Evaluation Study PT - Journal Article PT - Validation Study DEP - 20160513 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Environmental Pollutants) RN - 0 (Hydrocarbons, Aromatic) RN - DFC2HB4I0K (Polychlorinated Biphenyls) SB - IM MH - Animals MH - Environmental Pollutants/*analysis MH - Food Analysis/*methods MH - Food Contamination/*analysis MH - Humans MH - Hydrocarbons, Aromatic/*analysis/chemistry MH - Milk/*chemistry MH - Polychlorinated Biphenyls MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Solid Phase Extraction/*methods MH - Specimen Handling/methods MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - GC-HRMS OT - Human milk OT - PBDEs OT - PCBs OT - PCDD/Fs OT - POPs OT - Tandem SPE EDAT- 2016/05/15 06:00 MHDA- 2018/01/18 06:00 CRDT- 2016/05/15 06:00 PHST- 2016/01/26 00:00 [received] PHST- 2016/04/18 00:00 [accepted] PHST- 2016/03/24 00:00 [revised] PHST- 2016/05/15 06:00 [entrez] PHST- 2016/05/15 06:00 [pubmed] PHST- 2018/01/18 06:00 [medline] AID - 10.1007/s00216-016-9576-y [pii] AID - 10.1007/s00216-016-9576-y [doi] PST - ppublish SO - Anal Bioanal Chem. 2016 Jul;408(18):4897-906. doi: 10.1007/s00216-016-9576-y. Epub 2016 May 13.