|
| BFRs* | Sample matrix | Pretreatment | Extraction | Clean-up | Instrumental analysis | Recovery (%) | Reference |
|
| Di- to deca-BDEs, PBT, pTBX, PBEB, HBB, BTBPE, DBDPE, PBBs | Outdoor air | (i) GFF
(ii) PUF | (i) Soxhlet (48 hours)
(ii) Hexane/acetone (1 : 1) | (i) Silica/alumina column.
(ii) Elution with hexane-DCM (1 : 1) | GC-ECNI-MS | 67–122 ± 15% | [23] |
|
| Di- to deca-BDEs, BTBPE, DBDPE, PBEB, HBB | Outdoor air | (i) Quartz fibre filter
(ii) Amberlite XAD-2 resin. | (i) Soxhlet (24 hours)
(ii) Hexane/acetone (1 : 1) | (i) 3.5% (w/w) water-deactivated silica gel column.
(ii) Elution with 25 mL hexane followed by 25 mL hexane/DCM (1 : 1). | GC-ECNI-MS | 61–108 ± 19% | [24] |
|
| Tri- to deca-BDEs | Outdoor air | (i) GFF
(ii) PUF/XAD-2 resin. | (i) For GFF: ultrasonication with hexane/acetone (1 : 1) for 20 min. (3 times).
(ii) For PUF/XAD-2: Soxhlet (24 hours) using hexane/diethyl ether (8 : 2). | (i) Florisil cartridges topped with 0.5 g anhydrous Na2SO4 eluted with 8 mL hexane.
(ii) Multilayer column containing 1 g of each of H2SO4-impregnated silica (40% w/w), activated silica, and activated neutral alumina. Rinsed with 21 mL hexane (discarded). PBDEs were eluted with 15 mL hexane/DCM (8 : 2). | GC-ECNI-MS | 50–85 | [25] |
|
| Tri- to deca-BDEs, DPTE, HBB, TBPH, PBT, BTBPE, OBIND | Outdoor air | (i) GFF
(ii) PUF/XAD-2 resin. | (i) Soxhlet (16 hours)
(ii) hexane/DCM (1 : 1) | (i) 10% water deactivated silica column topped with 3 g anhydrous Na2SO4
(ii) Elution with 15 mL hexane | GC-ECNI-MS | 69–73 ± 12% | [26] |
|
| Tetra- to deca-BDEs, TBBP-A, α-, β- and γ-HBCDs | Indoor air (cars) | (i) GFF
(ii) PUF | (i) Soxhlet (8 hours)
(ii) DCM | (i) 8 g H2SO4-impregnated silica (44% w/w).
(ii) Elution with 25 mL hexane/DCM (1 : 1) | LC-APPI-MS/MS | 69–107 | [27] |
|
| Tri- to hepta-BDEs, hydroxyl-BDEs, methoxy-BDEs | Water, soil, sediment | | (i) Water: LLE with 25 mL (1 : 1) hexane/MTBE (twice)
(ii) Soil/sediment: 20 min ultrasonic extraction with 25 mL (1 : 1) hexane/MTBE followed by 10 min centrifugation (3 times) | (i) H2SO4-impregnated silica (preceded with 2 g Cu powder for sediment samples).
(ii) Elution with 40 mL DCM.
(iii) Fractionation on 5 g of 5% deactivated silica topped with 1 g anhydrous Na2SO4. | (i) GC-EI-MS for BDEs and methoxy-BDEs
(ii) LC-ESI-MS/MS for hydoxy-BDEs | 71–116 ± 14% | [28] |
|
| Tri- to deca-BDEs | Water | | SFOME using 25 μL 2-dodecanol as organic drop. | HPLC-UV | 81–116% | [29] |
|
| Mono- to hexa-PBBs | Water | |
(i) SPE using 100 mg of synthetic MIP loaded on silica gel
(ii) Elution with 3.0 mL hexane : DCM (1 : 1) | GC-ECD | 70–97 | [30] |
|
| Tetra- to deca-BDEs | Water, soil, sediment | (i) Water: filtered through 0.45 μm GFF, mixed with 40% methanol and sonicated for 30 min.
(ii) Soil/sediment: freeze-dried, sieved (0.2 mm mesh size), grounded, mixed with anhydrous Na2SO4 and dried. | (i) Water: SPE (C18 cartridges). Eluted with 3 mL methanol, 3 mL DCM, and 3 mL hexane.
(ii) Soil/sediment: MAE with 20 mL hexane/acetone (1 : 1) at 110°C for 20 min. | (i) Water: packed column with, from bottom to top, 6 cm alumina, 2 cm l silica, 5 cm alkalinized silica, 2 cm silica, 8 cm acidified silica, and 1 cm Na2SO4. Eluted with 70 mL DCM.
(ii) Soil/sediment: ultrasonication for 30 min with Cu powder for sulphur removal followed by sulphuric acid wash and florisil column. | GC-EI-MS | 53–130 | [31] |
|
| Tri- to deca-BDEs, HBCD, BTBPE, PBEB, and DBDPE. | Ice caps | XAD-2 resin columns. | Elution with methanol and DCM. | (i) 10% deactivated silica column. Eluted with 10% methanol in DCM.
(ii) Activated silica column. Eluted with hexane then (1 : 1) hexane: DCM. | GC-ECNI-MS | 76–93 ± 30% | [32] |
|
| Tetra- to deca-BDEs, TBBP-A, α-, β-, and γ-HBCDs | Dust (cars) | Sieving (500 μm mesh size). | PLE using hexane/DCM (1 : 9). Pressure 1500 psi, temp. 90°C, heating time 5 min, static time 4 min, 3 extraction cycles. | (i) 8 g H2SO4-impregnated silica (44% w/w).
(ii) Elution with 25 mL hexane/DCM (1 : 1) | LC-APPI-MS/MS | 71–105 | [33] |
|
| Tri- to deca-BDEs, α-, β-, and γ-HBCDs, BTBPE, DBDPE, HCDBCO, TBB, TBPH. | Dust
(house) | Sieving (500 μm mesh size). | (i) Vortexing with 2 mL hexane/acetone (3 : 1) for 2 min.
(ii) Ultrasonic extraction for 5 min. followed by centrifugation at 3500 rpm for 2 min (3 times). | (i) Florisil cartridge. Elution with 8 mL hexane (fraction1; BDEs, HBCDs, BTBPE, DBDPE, HCDBCO, TBB) then 10 mL EtAc (TBPH and HBCDs).
(ii) Fraction 1 is further cleaned up on H2SO4-impregnated silica (44% w/w). Elution with 10 mL hexane/DCM (1 : 1) | (i) GC-ECNI-MS
(ii) LC-ESI-MS/MS for HBCDs only. | 69–122 | [34] |
|
| Tri- to deca-BDEs | Dust (SRM) | Dust wet with DCM (2 : 3 w/w) | SFE using 1,1,1,2-tetrafluoroethane. 204 atm and 200°C. | | LC-APPI-MS/MS | 86 ± 6% | [35] |
|
| Di- to deca-BDEs, α-, β-, and γ-HBCDs, BTBPE, DBDPE | Soil | | (i) Shaking for 60 min with acetone/hexane (1 : 1)
(ii) Ultrasonication for 15 min
(iii) Centrifugation (2500 rpm, 10 min) | (i) Multilayer column (silica gel, 2% KOH-impregnated silica, 44% and 22% H2SO4-impregnated silica, Na2SO4). Eluted with hexane/DCM (3 : 1)
(ii) GPC | (i) GC-ECNI-MS
(ii) LC-ESI-MS/MS for HBCDs only. | 26–119 | [36] |
|
| Tri- to deca-BDEs | Soil | (i) Sieving (2 mm mesh size)
(ii) Dispersion in anhydrous Na2SO4
(iii) Air drying. | QuEChERS: vortexing for 2 min with 25 mL DCM followed by ultrasonication for 20 min the centrifugation at 5000 rpm for 5 min (2 times) | Alumina SPE cartridges. Elution with 6 mL DCM. | GC-ECNI-MS | 61–107 | [37] |
|
| Tetra- to hexa-BDEs | Sediment | (i) Freeze drying
(ii) Sieving (0.3 mm wire mesh) |
(i) SPME using polyacrylate coated fibre in the headspace mode at 100°C for 40 min.
(ii) Simultaneous oxidation with KMnO4 and H2SO4.
(iii) Thermal desorption of fibre at 300°C for 2 min. | GC-MS/MS | 76–111 | [38] |
|
| TBB, TBECH, TBCT, PBT, HBB, PBEB, PBBA, PBBB, HCDBCO, PBB153, α-, β-, γ-HBCDs, BTBPE, DBDPE | Sediment | (i) Air drying.
(ii) Dispersion in anhydrous Na2SO4 | (i) Soxhlet (24 hours)
(ii) Hexane/DCM (1 : 1) | (i) Cu powder to remove sulphur.
(ii) Multilayer column (activated silica, 40% H2SO4-impregnated silica, activated silica, anhydrous Na2SO4)
(iii) Elution with hexane/DCM (5 : 1) | GC-ECNI-MS | 79–87 ± 12 % | [39] |
|
| Tri- to deca-BDEs, HBB, BTBPE, TBB, TBPH | (i) Sludge
(ii) Biosolids
| Dispersion in anhydrous Na2SO4 | PLE using hexane/DCM (1 : 1). Pressure 1500 psi, temp. 100°C (3 cycles) | (i) GPC
(ii) Sulphuric acid wash. | (i) GC-EI-MS (HBB and BDE-209)
(ii) GC-ECNI-MS. | 79 ± 12% | [40] |
|
| Tri- to deca-BDEs, TBECH, PBT, HBB, PBEB, HCDBCO, TBB, TBPH, BTBPE, DBDPE | Sediment, sludge, dust | | UAE for 10 min with ethylacetate/cyclohexane (5 : 2). | Florisil columns and activated copper to remove sulphur from sediment samples. | GC-MS/MS | 69–140 | [41] |
|
