|
| BFRs* | Sample matrix | Pretreatment | Extraction | Clean-up | Instrumental analysis | Recovery (%) | Reference |
|
| PBBs (15, 31, 49, 52, 77, 101, 103, 153, 155, 169) | Fish tissue (trout, salmon, horse mackerel, sardine, and gilthead sea bream) | (i) Freeze drying
(ii) Equilibration overnight
(iii) Na2SO4 addition and mixing (3 : 1, w/w, ratio with sample)
(iv) Addition of 15 g of acidified silica (44%, w/w) | (i) PLE at 100°C with n-hexane
(ii) 3 static cycles of 5 min each and a flush volume of 60% | In-cell clean-up (see pretreatment) | GC-IT-MS/MS | 50–95% | [42] |
|
| PBDEs (28, 47, 66, 85, 99, 100, 153, 154, 183), MeO-PBDEs | Fish and shellfish | (i) Sample lyophilisation
(ii) Equilibration overnight
(iii) Addition of 25 g of activated Florisil (fat retainer) and 10 g of anhydrous Na2SO4 | (i) PLE at 100°C with DCM/n-hexane (1/9, v/v), 1500 psi
(ii) 3 static cycles of 5 min each and a flush volume of 100% | In-cell clean-up (see pretreatment) | GC-IT-MS/MS | 88–98%
90–98% | [43, 44] |
|
| HBCDs | Edible seaweed | Sample grinding | (i) PLE at 80°C with EtAc at 1500 psi
(ii) 2 static cycles of 3 min each and a flush volume of 60% | (i) Columns with neutral alumina (3% deactivated), neutral silica (3% deactivated), and Na2SO4
(ii) Elution with 25 mL n-hexane | LC-ESI-MS/MS | 93–103% | [45] |
|
| PBDEs (47, 99, 100, 153) | Fish | Sample grinding with anhydrous Na2SO4 | US extracted for 30 min with 8 mL of DCM/n-hexane (1/4, v/v) | Extract mixed with C18-silica, vortexed, and centrifuged | GC-EI-MS/MS | 75–114% | [46] |
|
| PBDEs (47, 99, 100, 85, 154, 153) | Plastic bottled beverages | Degassed for 10 min in an ultrasonic bath at ambient temperature | Dispersive solid-phase extraction with 4 mL acetonitrile, with 6 g of anh MgSO4 and 1.5 g of NaCl | Dispersive liquid-liquid microextraction with 50 mg primary amine silica (PSA) for green tea beverage, 50 mg C18 for carbonated beverage, and a mixture of 50 mg PSA and 25 mg C18 for orange juice | GC-EI-MS | 85–115% | [47] |
|
| PBDEs (47, 85, 99, 100, 153, 154) | Milk (supermarket
and raw bovine milk) | (i) 5 mL of 50% (w/v) NaOH and 1 mL of acetone
(ii) The mixture was further heated at 70°C in water bath | Dispersive liquid-liquid microextraction with 5 mL n-hexane | LC-Florisil column: elution with n-hexane, solvent exchanged to acetone and water and further extracted in chlorobenzene | GC-EI-MS | 73–98% | [48] |
|
| PBDEs, HBCDs, PBT, HBB, PBEB, BTBPE, DBDPE | Chicken eggs | Lyophiliztion | Soxhlet extraction with hexane/acetone (1 : 1) for 48 h | (i) Gel permeation chromatography
(ii) Multilayer silica gel column packed with neutral silica and acidified silica. | GC-ECNI-MS | 84–138% | [49] |
|
| 17 PBDEs and 30 NBFRs | Blubber of harbour porpoises | | PLE with hexane/acetone (1 : 1) at 100°C and 120 bar. | (i) Gel permeation chromatography
(ii) Florisil column | GC-MS/MS | 70–120% | [50] |
|
| PBDEs (3, 15, 28, 47, 77, 99, 100, 118, 126, 153, 183) | Venous and umbilical cord blood sera (human) | Addition of 3 mL of concentrated H2SO4 | Multiple liquid-liquid extraction with n-hexane
(total of 7 mL solvent) | Addition of 2 mL of concentrated H2SO4 | GC-ECNI-MS | 90–120% | [51] |
|
| PBDEs (47, 99, 100, 153, 183) | (i) Human blood (50 µL)
(ii) Dried blood spot (human) | (i) 2 h for equilibration, formic acid : acetone (3/2, v/v) for protein denaturation.
(ii) Cut into small pieces, formic acid : acetone (2/3, v/v) for protein denaturation. | (i) LLE with DCM/n-hexane (1/4, v/v) and repeated with n-hexane followed by combination of organic solvents.
(ii) ultrasonication with DCM/n-hexane (4/1, v/v) and repeated with n-hexane followed by combination of organic solvents. | | GC-EI-HRMS | (i) 71–99
(ii) 75–120% | [52] |
|
| TBBP-A, α-, β-, and γ-HBCDs | Human milk | Freeze-drying | PLE using hexane/DCM (1 : 9). Pressure 1500 psi, temp. 90°C, heating time 5 min, static time 4 min, 3 extraction cycles. | (i) Wash with concentrated sulphuric acid.
(ii) Florisil/Na2SO4 column. | LC-MS/MS | 78–109% | [43] |
|
| PBDEs (47, 85, 99, 100, 153, 154, 183, 196, 197, 203, 206, 207, 208, 209) | Human milk | Freeze-drying | PLE using hexane/DCM (1 : 9). Pressure 1500 psi, temp. 90°C, heating time 5 min, static time 4 min, 3 extraction cycles. | (i) Wash with concentrated sulphuric acid.
(ii) Florisil/Na2SO4 column. | LC-MS/MS | 74–112% | [53] |
|
