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.

The impact of environmental pollution on the quality of mother's milk

“…The dominant method used for detection and identification of polychlorinated biphenyls and dioxins is gas chromatography with electron capture detector (Hassine et al 2012 ; Polder et al 2008 ; Skrbić et al 2010 ), and mass spectrometry (Bencko et al 2004 ; Černá et al 2010 ; Chovancová et al 2011 ; Deng et al 2012 ; Ryan and Rawn 2014 ; Schuhmacher et al 2007 ; Vigh et al 2013 ; Zhang et al 2016 ). Techniques used for sample preparation include classical liquid-liquid extraction (LLE) (Bencko et al 2004 ; Černá et al 2010 ; Chovancová et al 2011 ; Hassine et al 2012 ; Ryan and Rawn 2014 ), solid phase extraction (SPE) (Dmitrovic and Chan 2002 ; Lin et al 2016 ), and accelerated solvent extraction (ASE) (Deng et al 2012 ; Vigh et al 2013 ; Zhang et al 2016 ). It is important to improve the sample preparation stage and search for a method which will make it possible to analyze a lot of samples in a short time, with small amounts of solvents.…”

The new Israeli feed safety law: challenges in relation to animal and public health

“…The method of choice for the combined confirmation of dioxins and dioxin‐like PCBs is gas chromatography‐high resolution mass spectrometry after an extensive sample clean‐up procedure . Dioxin‐like compounds such as PCBs can also be determined by GC with other low resolution mass spectrometry instruments such as GC‐MS.…”

QuEChERS extraction coupled to GC-MS for a fast determination of polychlorinated biphenyls in breast milk from Polish women

“…Human milk is a very heterogeneous matrix, which needs a specific method of sample cleanup. Classical liquid-liquid extraction (LLE) (Bencko et al 2004; Hassine et al 2012) and solid-phase extraction (SPE) (Lin et al 2016) are typical methods used for isolation of PCBs from samples. To minimize use of hazardous solvents as well as the cost and time of sample preparation, it is important to improve this stage of analysis, also with a view to obtaining better results for specific types of analytes and matrices.…”