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. 2022 Feb 9;19(4):1935. doi: 10.3390/ijerph19041935

Table 2.

Methodologies applied in reviewed articles (NR—not reported, Y—substances included in the study, N—substances not included in the study).

Pre-Deployment Post-Deployment Extraction Post-Extraction Sample Cleanup Analyzed Substances Instrumental Analysis
Publication Year Mechanism Protocol Mechanism Protocol Mechanism Protocol Instrumentation Protocol NBRFs OPEs PAHs BFRs PCBs PEs Pesticides PPCPs Other Ref.
2014 Agitated wash (orbital shaker) 3 × EtAc:n-hex (2.5 h), 60 rpm
2 × EtAc:MeOH (2.5 h), 60 rpm
Rinse 2 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc,100 mL, (2 h), 60 rpm NR NR N Y Y N Y Y Y Y Y GC-MS [20]
2016 Thermal conditioning 280–300 °C (48 h) Rinse 1 × DI water
1 × IPA
NR 2 × EtAc, 100 mL NR NR N N N N N N Y N N GC-ECD [55]
2016 Soxhlet extraction 1 × EtAc:n-hex, (12 h)
1 × EtAc:MeOH, (12 h)
NR NR Soxhlet extraction 1 × n-hex:acetone, (12 h) Syringe filter (0.2 µm PTFE)
SPE cartridges (Florisil, 500 mg)
Filtration
Elution:
N Y N N N N N N N GC-MS [51]
F1:n-hex (10 mL)
F2:EtAc (10 mL)
2017 Wash 3 × EtAc:n-hex
2 × EtAc:MeOH
Rinse 2 × DI water
1 × IPA
Wash 1 × EtAc, 100 mL, (12 h)
1 × EtAc, 100 mL, (2 h)
NR NR Y Y Y Y Y Y Y Y Y GC-ECD, GC-MS [19]
2017 Conditioning (vacuum oven) 300 °C, 180 min, 0.1 Torr Rinse 2 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc, 100 mL NR NR N Y Y Y Y N Y Y Y GC-MS, GC-MS/MS, GC-µECD [36]
2017 Soak EtAc, n-hex, MeOH Rinse 2 × water
1 × IPA
NR 2 × EtAc, 100 mL SPE cartridges (C18, 500 mg) Elution: ACN Y Y N Y N N N N N GC-MS [52]
2018 NR NR Rinse 1 × DI water
1 × IPA
Dialysis 2 × EtAc NR NR N N Y N N N N N N GC-MS/MS [57]
2018 Solvent exchange 3 × EtAc:n-hex
2 × EtAc:MeOH
Rinse 2 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc 100 mL, 60 rpm NR NR N N Y N N N N N N GC-MS/MS [48]
2018 Agitated wash (overhead shaker) 1 × EtAc:n-hex, (30 min)
1 × EtAc:MeOH, (30 min):
NR NR Agitated wash (overhead shaker) 2 × EtAc, 40 mL, (30 min) NR NR N N N N N N Y N N LC-MS [24]
2018 NR NR Rinse 2 × DI water
1 × IPA
Wash 1 × EtAc 100 mL, (12 h)
1 × EtAc, 100 mL, (2 h)
NR NR N N N N N N Y N N GC-µECD [27]
2018 Soxhlet extraction 1 × EtAc:n-hex, (12 h)
1 × EtAc:MeOH, (12 h)
NR NR Sonication 3 × n-hex:acetone, 10 mL Custom SPE: Florisil (500 mg) and silica gel (12 g; F1 only) Elution (Florisil): Y N N Y N N N N N GC-MS [58]
F1:n-hex
F2:EtAc
Elution (silica gel):
F3:DCM:n-hex
2019 Rinse, conditioning Water rinse, thermal conditioning Rinse 1 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc, 100 mL, (2 h) NR NR NR NR NR NR NR NR NR NR NR GC-MS [67]
2019 Soxhlet extraction 1 × EtAc:n-hex, (24 h)
1 × EtAc:MeOH, (24 h)
NR NR Sonication 2 × n-hex:acetone, 30 mL, (2 h) Custom SPE (neutral alumina, neutral silica gel, sulfuric acid- silica gel, sodium sulfate) Elution: DCM (40 mL) Y Y N Y N N N N Y GC-MS [21]
Custom SPE (neutral alumina, neutral silica, Florisil, sodium sulfate) Elution:
F1:DCM (40 mL)
F2:EtAc (40 mL)
2019 NR NR Rinse 2 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc, 100 mL, 60 rpm NR NR N Y Y N N Y Y Y Y GC-MS [59]
2019 Thermal conditioning (vacuum oven) 300 °C, (180 min), 0.1 Torr Rinse 1 × DI water
1 × IPA
NR 2 × EtAc, 100 mL SPE (C18, silica) Elution: ACN Y Y Y Y Y Y Y Y Y GC-µECD, GC-MS [61]
2019 Soak EtAc, n-hex, MeOH NR NR NR 2 × EtAc, 100 mL SPE cartridges (C18, 500 mg) Elution: ACN N Y N N N N N N N GC-MS [62]
2019 Soxhlet extraction Agitated wash 1 × DI water Sonication 1 × Acetone:n-hex, 20 mL, (2 h) Custom SPE (neutral alumina, neutral silica, Florisil, anhydrous sodium sulfate) Elution: Y Y Y Y N N N N Y GC-MS [63]
F1:DCM
F2:EtAc
Rinse 1 × IPA Custom SPE, (neutral alumina, neutral silica, acidic silica, anhydrous sodium sulfate) elution:
F3: DCM
2019 NR NR Rinse 2 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc, 100 mL, (2 h), 60 rpm - - N N Y N N Y Y N Y GC-GC/ToF-MS [45]
2020 Soxhlet extraction 1 × EtAc (3 days) - - Agitated wash (Wrist Action Shaker) 1 × ACN, 30 mL Syringe filter (0.2 µm, Teflon) Filtration Y Y N Y N N N N Y GC-MS [49]
2020 Agitated wash (platform shaker) 3 × EtAc:n-hex, (2.5 h)
2 × EtAc:MeOH, (2.5 h), 60 rpm
NR NR Agitated wash (orbital shaker) 2 × EtAc, 25 mL, (2 h), 60 rpm SPE cartridges (C18, 500 mg) Elution: ACN Y Y N Y Y N Y N Y GC-MS [68]
2020 NR NR Rinse 1 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc, 25 mL, (24 h) SPE cartridges (C18, 500 mg) Elution: n-hex: DCM (4 mL) N N Y N N N N Y N GC-MS [69]
2020 Agitated wash (orbital shaker) 1 × MeOH (10 min)
3 × n-hex:EtAc (1 h),
2 × MeOH:EtAc
Rinse 1 × MeOH agitated wash (orbital shaker) 2 × 30 mL EtAc, 30 mL, (1 h) NR NR N N Y N N N N N N GC-MS [18]
2020 Soxhlet extraction 1 × EtAc:n-hex, (12 h)
1 × EtAc:MeOH, (12 h)
NR NR Sonication 3 × n-hex: DCM, 10 mL, (15 min) SPE (Florisil, 8 g) Elution: N Y N N N N N N N GC-MS/MS [70]
F1:n-hex
F2:EtAc
2020 Soxhlet extraction 1 × EtAc:n-hex, (24 h)
1 × EtAc:MeOH, (24 h)
NR NR Sonication 2 × n-hex:acetone, 30 mL, (2 h) Custom SPE (neutral alumina, neutral silica, Florisil, sodium sulfate) Elution: DCM N N Y N N N N N N GC-MS [47]
2020 Agitated wash (orbital shaker) 2 × MeOH, (10 min), 120 rpm
2 × (1 h): n-hex:EtAc, (1 h), 120 rpm
2 × MeOH:EtAc, 120 rpm
Rinse 1 × MeOH Agitated wash (overhead shaker) 2 × EtAc, 30 mL NR NR N N Y N N N N N N GC-MS [71]
2020 Conditioning (vacuum oven) 300 °C, (12 h), 0.1 Torr Rinse 2 × DI water
1 × IPA
NR 2 × EtAc, 50 mL SPE cartridges (C18) Eluted: ACN N Y Y Y Y Y Y Y Y GC-MS [46]
2020 Soxhlet extraction 1 × EtAc:n-hex, (12 h)
1 × EtAc:MeOH, (12 h)
NR NR Sonication 3 × n-hex:DCM, 10 mL) SPE cartridges (Florisil, 500 mg) Elution: N Y N N N Y N N Y GC-MS [72]
F1: n-hex
F2: EtAc
F3: MeOH
2020 NR NR Rinse DI water Sonication 2 × n-hex: acetone, 30 mL, (2 h) Chromatography column (neutral alumina, neutral silica gel, sulfuric acid-silica gel, sodium sulfate) Elution: DCM Y Y Y Y N N N N N GC-MS [28]
Chromatography column (neutral alumina, neutral silica gel, Florisil, sodium sulfate) Elution:F1:DCM
F2:EtAc
2020 Soxhlet extraction 1 × pentane (3 days) - - Agitated wash ACN SPE cartridge (Florisil, 500 mg) Elution: EtAc Y Y N Y N N N N Y GC-MS [73]
2020 Agitated wash (magnetic stir plate) 3 × EtAc:n-hex, (30 min), 60 rpm
2 × EtAc:MeOH, (30 min), 60 rpm
NR NR Agitated wash (magnetic stir plate) ACN:MeOH, 20 mL, (1 h), 60 rpm NR NR N N N N N N N N Y HPLC [65]
2020 NR NR NR NR Sonication 3 × n-hex:DCM, 10 mL SPE (Florisil, 8 g) Elution: Y Y N Y Y Y Y N Y GC-MS, GC-MS/MS [74]
F1: n-hex,
F2: EtAc,
F3: MeOH
2020 Agitated wash (orbital shaker) 1 × MeOH (10 min), 120 rpm
2 × EtAc:n-hex (1 h), 120 rpm
2 × EtAc:MeOH (1 h), 120 rpm
NR NR Agitated wash (orbital shaker) 2 × EtAc, 30 mL, (1 h), 120 rpm NR NR N N Y N N N N N N GC-MS [75]
2021 Soxhlet extraction 1 × EtAc:n-hex (12 h)
1 × EtAc:MeOH (12 h)
NR NR Sonication 3 × DCM:n-hex SPE cartridges (Florisil, 500 mg) Elution: N N N N N N N Y Y LC-MS [76]
F1
F2: EtAc
F3
2021 Rinse, conditioning DI water, 300 °C (180 min) rinse 1 × DI water
1 × IPA
Agitated wash (orbital shaker) 2 × EtAc SPE (C18, silica) Elution: ACN N N N N N N Y N N GC-ECD, GC-MS [77]
2021 Sonication 3 × DCM:n-hex, (20 min) NR NR Sonication 2 × DCM: n-hex, 15 mL, (20 min) SPE cartridges (Florisil, 2 g) Elution:
1 × n-hex
1 × EtAc
N Y N N N N N N N LC-MS [78]

Abbreviations: ACN, acetonitrile; BFRs, brominated flame retardants; DCM, dichloromethane; DI, deionized; EtAc, ethyl acetate; F1, F2, F3, numeration of fractions eluted (in accordance to their order of elution); IPA, isopropyl alcohol; MeOH, methanol; NBFRs, novel brominated flame retardants; n-hex, n-hexane; OPEs, organophosphate esters; PAHs, polycyclic aromatic hydrocarbons; PCBs, polychlorinated biphenyls; PEs, phthalate esters; PPCPs, pharmaceuticals and personal care products; SPE, solid phase extraction.