Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in fishery and aquaculture products using sequential solid phase extraction and large volume injection gas chromatography/tandem mass spectrometry

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

“…The lab-made SPE cartridges used were prepared according to our previous study [19]. Briefly, silica gel, basic alumina, and anhydrous sodium sulfate were rinsed with dichloromethane (20 mL per g) and then activated/baked under the condition of 180°C for 1 h, 600°C for 24 h, and 400°C for 1 h, respectively.…”

“…The traditional sample pretreatment method, based on a Soxhlet extraction and a cleanup through multiple chromatographic columns using silica, acid silica, florisil, and alumina as adsorbents, has limited use because of its well-known disadvantages in manual operation, much time and organic solvent consuming, and large deviations (e.g., QC and measured results) frequently occurred from batch to batch or even from sample to sample in the same batch [10,[14][15][16][17][18][19]]. An integrated method, based on accelerated solvent extraction (ASE) of lyophilized human milk, defatting based on the sulfuric acid silica gel, and cleaning up with a fluid management system (FMS, based on acid multilayer silica, basic alumina, and carbon columns) [4,14,18,20,21], or a FMS liked technique-automate sample clean-up system (ASCS, with the same columns as FMS) [8], has been widely adopted in sample pretreatment with the characters of high effectiveness and automation.…”

“…An integrated method, based on accelerated solvent extraction (ASE) of lyophilized human milk, defatting based on the sulfuric acid silica gel, and cleaning up with a fluid management system (FMS, based on acid multilayer silica, basic alumina, and carbon columns) [4,14,18,20,21], or a FMS liked technique-automate sample clean-up system (ASCS, with the same columns as FMS) [8], has been widely adopted in sample pretreatment with the characters of high effectiveness and automation. However, the cleanup method via FMS or ASCS would use large amounts of solvents to quantitatively recover analytes and remove crosscontamination by washing with extra solvents [14,18,19]. Additionally, the method still lacks high throughput, and each instrument only treats a sample in each batch (in total at least 4 h needed for chromatographic column conditioning, sample loading, washing and eluting, and finally post-washing), which also generates high cost in the use of solvents and commerical chromatographic columns.…”

“…Additionally, the method still lacks high throughput, and each instrument only treats a sample in each batch (in total at least 4 h needed for chromatographic column conditioning, sample loading, washing and eluting, and finally post-washing), which also generates high cost in the use of solvents and commerical chromatographic columns. A tandem solid phase extraction (SPE) based on sulfuric acid silica cartridge coupled with basic alumina cartridge was developed for the determination of PCBs and PBDEs in fishery and aquaculture products with many advantages over ASCS method [19]. The mean lipid content of human milk is about 5 % and comparable to that of the common fish.…”

Determination of Nine Hydroxylated Polybrominated Diphenyl Ethers and Forty Polybrominated Diphenyl Ethers in Atmospheric Fine Particles by Precolumn Derivatization-GC-MS/GC

“…Currently the main pretreatment methods for analyzing different polarity fractions require several steps, including extraction, separation and clean-up. Numerous techniques have been developed for extracting analytes, such as accelerated solvent extraction (ASE) [12], Soxhlet…”