title: 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.
abstract: 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.
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China.
authors.forename: Yuanjie
authors.initials: Y
authors.lastname: Lin
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China.
authors.forename: Chao
authors.initials: C
authors.lastname: Feng
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China.
authors.forename: Qian
authors.initials: Q
authors.lastname: Xu
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. ludasheng@scdc.sh.cn.|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.
authors.forename: Dasheng
authors.initials: D
authors.lastname: Lu
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China.
authors.forename: Xinlei
authors.initials: X
authors.lastname: Qiu
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China.
authors.forename: Yu'e
authors.initials: Y
authors.lastname: Jin
authors.affiliation: Shanghai Municipal Center for Disease Control and Prevention, 1380 Zhongshan West Road, Shanghai, 200336, China. wangguoquan@scdc.sh.cn.
authors.forename: Guoquan
authors.initials: G
authors.lastname: Wang
authors.affiliation: California Department of Public Health, 850 Marina Bay Parkway, Richmond, CA, 94804, USA.
authors.forename: Dongli
authors.initials: D
authors.lastname: Wang
authors.affiliation: California Department of Public Health, 850 Marina Bay Parkway, Richmond, CA, 94804, USA.
authors.forename: Jianwen
authors.initials: J
authors.lastname: She
authors.affiliation: 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.
authors.forename: Zhijun
authors.initials: Z
authors.lastname: Zhou
mesh_terms: D000818:Animals; D004785:Environmental Pollutants / Q000032:analysis*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D006801:Humans; D006841:Hydrocarbons, Aromatic / Q000032:analysis* / Q000737:chemistry; D008892:Milk / Q000737:chemistry*; D011078:Polychlorinated Biphenyls; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D013048:Specimen Handling / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D004785:Environmental Pollutants; D006841:Hydrocarbons, Aromatic; D011078:Polychlorinated Biphenyls
keywords: GC-HRMS; Human milk; PBDEs; PCBs; PCDD/Fs; POPs; Tandem SPE