Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples
Abstract
:1. Introduction
2. Modes and Variations of Liquid-Phase Microextraction
Technique | Solvent properties | Solvent volume | Sample preparation; other equipment | Mixing/ stirring | Extraction time | Typical analytes | Automation | Other considerations & modifications |
---|---|---|---|---|---|---|---|---|
SDME | immiscible with water; usually GC-compatible HS-SDME: low vapor pressure, also water; recent: ionic liquids | 1–8 µL | GC syringe sample: filtration in DI-SDME; adjustment of ionic strength, T | DI-SDME: up to 600 rpm HS-SDME: higher rates | min. 1–15 min, usually longer | non-polar, semi-volatile or volatile (HS-SDME) | semi-automatic in dynamic mode; continuous flow ME (CF-ME) [34] | simple; ready-to-analyze extracts; modifications: dynamic mode possible in-needle or in-syringe; LLLME with back-extraction into droplet of 2nd immiscible solvent; exhaustive extraction by multiple HS-SDME [35] |
HF-LPME | immiscible with water; compatible with HF material; low volatility & viscosity, e.g., toluene, n-octanol, also di-n-hexyl ether HF-LLLME: above valid for solvent in the HF wall; in the HF lumen: aqueous acceptor phase or ionic liquid or immiscible organic solvent | 4–20 µL | small-diameter porous tube (fiber), usually polypropylene, one end sealed, other attached to syringe sample: adjustment of pH and ionic strength | vigorous stirring or vibration, microwaves | 20–60 min (except for dynamic HF-LPME or EME) | non-polar; ionizable (in HF-LLLME) | yes, with autosampler; dynamic HF-LPME [36]; still each fiber manually prepared | applicable to »dirty« samples; modifications: dynamic HF-LPME [36]; solvent-bar microextraction (SBE) [37]; air in HF wall with aqueous solvent in lumen for volatile analytes [38] |
DLLME | disperser solvent: miscible with water, e.g., acetone, methanol, ethanol, acetonitrile, THF; extraction solvent: ρsolv. > ρaq, e.g., C2Cl4, Cl-benzene, CH2Cl2, CHCl3, CCl4, ionic liquid; OR ρsolv. < ρaq, e.g., 1- or 2-dodecanol, 1-undecanol, hexadecane (Tmp ≈ room T), also cyclohexane, n-hexanol, tri-n-butyl-phosphate | Disp.s.: 0, 1–2 mL Extr.s.: 10–150 µL | centrifuge (ρsolv. > ρaq); ice bath or special extracting vessel (ρsolv. < ρaq); sample: filtration, adjustment of pH and ionic strength | not needed; ultrasound, vortex [9] | equilibration in few seconds; phase separation 1–20 min | non-polar | barely possible, although attempts [39] | modifications: temperature-controlled DLLME with ionic liquids, mixing and separation of phases at high/low T [40] |
LPME | Analytical techn. | Sample | Analytes | Extraction procedure for solid sample | Optimized extraction conditions for s.s. | LPME procedure | Method performance | Ref. |
---|---|---|---|---|---|---|---|---|
DLLME | GC-ECD | soil | 5 PCBs | 1 g s.s. + 10 mL AC; mech. shaking 30 min; upper layer | extraction solvent | 1.0 mL AC extract (DS) + 30 µL Cl-benzene (ES) inj. into 5.0 mL w.; centrif.; sedim. phase evaporated, rediss. in 20 µL n-hexane | η 82.3%–113.6% (3 levels); RSD < 6.4%; LOD 0.20–0.50 ng/g | [60] |
US-DLLME | GC-MS (SIM) | soil | endosulfan & 5 metab. | 0.5 g s.s. + 1.25 mL AC; US (10 min); centrif. | not given | AC extract (DS) + 58 μL TCE (ES) inj. into 5.0 mL w. + 7% Na2SO4; US (2 min); centrif.; direct injection | experimental design for US-DLLME optimization; η 89.0%–99.7%; RSD < 6.3%; LOD 0.316–2.494 ng/g; no interference from sample matrix observed | [61] |
DLLME | HPLC-FLD | sediment | PAHs | 0.2 g s.s. + 2 mL ACN, VA (2 min), centrif. | extraction solvent, vortex time | 1.0 mL ACN extract (DS) + 80 μL CH2Cl2 (ES) inj. into 5.0 mL w.; centrif.; sedim. phase evaporated, rediss. in 40 μL ACN | η 72.9%–97.8% (3 levels); RSD < 8.0%; LOD 2.3–6.8 ng/g; no interference from sample matrix observed | [62] |
DLLME | LC-FLD | soil | carbaryl, triazophos | 1 g s.s. + 10 mL MeOH, mech. shaking (30 min); filtered | extraction solvent | 1.0 mL MeOH extract (DS) + 50 µL TtCE (ES) inj. into 5.0 mL w.; centrif.; sedim. phase evaporated, rediss. in 25 μL MeOH | η 80.8%–111.1% (3 levels); RSD < 4.3%; LOD 0.014–0.110 ng/g; some matrix interferences present in chromatograms | [63] |
US-IL-DLLME | HPLC-UV | soil | 3 pesticides | 10 g s.s. + 30 mL sol. (60% MeOH, 5 mg NaCl); US, centrif. + filtr.; repeat; evaporated to dryness, rediss. in 10 mL MeOH sol., pH adjust to 4.0 | not given | 1.0 mL sample sol., inj. 0.3 mL MeOH (DS) + 70 μL [BMIM]TFSI (ES); shake, US (2 min); centrif.; sedim. phase dissolved in 0.5 mL MeOH | not given for overall method (just for DLLME) | [64] |
IL-DLLME | HPLC-FLD | soil | 5 pesticides 2 metabol. | 3 g s.s. + 20 mL MeOH + 2.5% NaCl; manual shaking + US; centrif. + filtr.; repeat; evaporated to dryness, rediss. in 10.0 mL w., pH adjust to 5.2 | extraction solvent, Vsolv, NaCl add., US time, amount of sample | add. NaCl to 30%; MeOH (DS) + IL ([HMIm][PF6], ES); centrif.; 80 µL sedim. phase dissolved in 1120 µL ACN-phosphate buffer | central composite experimental design for optimization of IL-DLLME conditions; η 88%–119%; LOD 0.02–27.1 ng/g | [65] |
IL-DLLME | HPLC-FLD | soil | 7 pesticides and metabol. | 3 g s.s. + 20 mL MeOH + 2.5% NaCl; manual shaking + US (10 min), centrif. + filtr.; repeat; evaporated to dryness, rediss. in 10.0 mL w., pH adjust to 5.2 | not given | comparison of 2 IL as ES: [PPIm][PF6] and [HMIm][PF6]; add. NaCl (2.5 g); MeOH (DS) 418 μL + IL 117.5 mg (ES); VA 1 min; centrif.; 80 µL sedim. phase dissolved in 1120 µL ACN-phosphate buffer | η 93%–118%; RSD < 20%; LOD 0.02–60.5 ng/g | [66] |
DLLME | sweeping MEKC-DAD | soil | 5 sulfonylurea herbicides | 10 g s.s. + 10 mL ACN (5% HCOOH, pH 3.0), shaking; added 4 g MgSO4 + 1 g NaCl, shaking; centrif.; 5 mL supernatant + 250 mg C18 + 1.5 g MgSO4, shaking; centrif., filtered | extraction solvent, pH of sample solution for DSPE, DSPE sorbent | 1.0 mL extract (DS) + 50 µL ClBz inj. into 5.0 mL w. (pH 2.0, HCl), VA (5 s); centrif.; sedim. phase evaporated, rediss. in 20.0 µL phosphate buffer (pH 10.0) | η 76.0%–93.5% (3 levels); RSD < 6.8%; LOD 0.5–1.0 ng/g | [67] |
DLLME | HPLC-DAD | soil | 4 sulfonylurea herbicides | 10 g s.s. + 20 mL AC/0.15 M NaHCO3 (2:8), shaking 30 min; filtered; 10 mL filtrate + 0.15 g C18, shaking 5 min; filtered; pH adj. to 2.0 and dil. to 25 mL with AC/w. (2:8, pH 2.0) | organic solvent, DSPE sorbent | 5.0 mL solution (with AC 20% as DS) + 60 µL ClBz (ES), VA 5 s; centrif.; sedim. phase evaporated, rediss. in 15 µL ACN | η 78.0%–92.5% (3 levels); RSD < 7.2%; LOD 0.5–1.2 ng/g; some interferences present in chromatograms | [68] |
DLLME | GC-MS/MS | sediment | 4 PBDEs | 0.25 g s.s. + 1.5 mL AC; US (35 °C) 6 × 5 min; centrif.; 1.2 mL leachate + 100 mg SiO2, VA (30 s); centrif. | leaching solvent, Vsolv, DSPE sorbent, US time & mode, US-transmitting liq., leaching T | 1.0 mL AC extract (DS) + 60 µL CCl4 (ES) inj. into 5.0 mL w.; shaking, 5 min in bath (35 °C); centrif.; direct injection | η 80%–112% (2 levels); RSD < 9.8%; LOD 0.02–0.06 ng/g; extraction method comparable efficiency with Soxhlet's | [69] |
DLLME | GC-MS/MS | sediment | 4 PBDEs | 1 g s.s. + 1.2 mL MeOH; US (40 °C) 2 × 9.2 min; centrif. | leaching solvent type (also a DS) & V, T, US time & cycles | 0.1 mL MeOH (DS) + 22 mg 1-dodecanol (ES) inj. into 0.4 mL leachate + 1.0 mL 6.15 M NaCl + 4.4 mL w. at 40 °C; SFOD form. at 10 min in ice bath; collected, melt, add. 3 µL i-octane; direct injection | factorial (2k) screening & central composite design for optimization; η 71%–104% (2 levels); RSD < 9.2%; LOD 0.5–1.8 pg/g | [70] |
HLLE | GC-ECD | soil | 3 organo-phosph. & pyrethroid pesticides | 4.0 g s.s. + 10 mL AC; mech. shaking (30 min); supernatant decanted | extraction solvent, Vsolv | 1.0 mL AC extract (CS) + 40 µL CCl4 (ES) inj. into 5.0 mL w.; phase separation by 0.3 g NaCl; centrif.; direct injection | η 79.2%–113.1%; RSD < 9.6%; LOD 0.01–0.04 ng/g | [71] |
USA-EME | GC-FID | soil | diazinon, chlorpyrifos | 2 g s.s. + 2.5 mL MeOH; US (2 min pulse on/off); centrif., filtered | not given | 1.5 mL extract + 10.5 mL w.; 14 µL toluene slowly injected during US, US (30 s); centrif.; upper phase collection, direct injection | η 90.0%–105%; RSD < 9.2%; LOD not given for soil; several interferences in the chromatogram | [72] |
HF-LPME | GC-ICP-MS | soil, dust | 4 PBDEs | 0.5 g soil/0.05 g dust + 3 mL MeOH; US (30 min); centrif.; supernatant diluted to 10 mL with w. | not given | 3.0 mL extract, 4 µL decane (ES) in 1.5-cm HF; stirring 20 min at 40 °C & 1000 rpm; direct injection | η 86.7%–110.9%; RSD < 10.4%; LOD not given for soil & dust; several interferences present in the chromatogram (brominated compounds?) | [73] |
HF-LPME | GC-ECD | sediment | vinclozoline | 5 g s.s. + 10 mL ACN-MeOH (9:1); US 30 min; centrif., evapor. to 0.05 mL | extraction solvent | extract + 5 mL w., 3 µL toluene (ES) in 1.3-cm HF; stirring 20 min at 800 rpm; direct injection | η 94%–96% (2 levels); RSD 6.1%; LOD 0.5 ng/g | [74] |
HF-LPME | HPLC-FLD | soil | 7 pesticides and metabol. | 3 g s.s. + 20 mL MeOH + 2.5% NaCl; manual shaking + US (10 min); centrif. + filtr.; repeat; evaporated to dryness, rediss. in 10.0 mL w., filtered | not given | extract (pH adj. to 9.0, NaCl to 20%), 20 µL 1-octanol (ES) in 2.0-cm HF; stirring 30 min at 1440 rpm; ES evaporated, rediss. in 50 µL mobile phase for HPLC | η 85%–117%; RSD variable, up to 71% at low levels; LOD 0.001–6.94 ng/g | [75] |
HF-LLLME | GC-ECD | soil | chlorophenols | 2 g s.s. + 3 mL MeOH; US (2 min pulse on/off); centrif., filtered | not given except for MeOH effect on HF-LLLME | 2 mL extract dil. to 20 mL with w., dodecane in 8-cm HF wall (ES) & 25 µL ACN (AS) + IS in HF lumen; stirring 30 min at 400 rpm; direct injection | η 86.3%–110%; RSD < 9.3%; LOD not given for soil | [58] |
HF-LLLME, dynamic | GC-FID | soil | PAHs | 2 g s.s. + 3 mL MeOH; US (2 min pulse on/off); centrif., filtered | not given except for MeOH effect on HF-LLLME | 2 mL extract dil. to 20 mL with w. + dodecane in 8-cm HF wall (ES) & 25 µL ACN (AS) in HF lumen; stirring 20 min at 1000 rpm; dynamic extr. (syringe plunger); direct injection | η 84.4%–110%; RSD < 9.3%; LOD not given for soil | [36] |
3. Liquid-Phase Microextraction Applied to (Semi)Solid Environmental Samples as a Step for Preconcentration and Clean-up of Extracts
3.1. LPME Combined with Conventional Solvent Extraction
LPME | Analytical techn. | Sample | Analytes | Extraction procedure for solid sample | Optimized extraction conditions for s.s. | LPME procedure | Method performance | Ref. |
---|---|---|---|---|---|---|---|---|
US-DLLME | GC-ECD | soil | 3 pyrethroids | MSPD: 0.1 g s.s. + 0.3 g SiO2 (d 38 µm) blended in mortar; transf. to cartridge with 0.1 g Na2SO4(anhyd); eluted with 3 mL AC; evaporated to 0.5 mL | sorbent, sample/sorb. ratio, eluting solv. type and V, | AC extract (DS) + 50 µL TtCEt (ES) inj. into 5 mL w.; US 2 min; centrif.; sedim. phase evaporated, rediss. in 20 µL n-hexane | η 83.6%–98.5%; RSD < 7.3%; LOD 0.45–1.13 ng/g | [77] |
DLLME | HPLC-FLD | soil | carbendazime thiabendazole | 20 g s.s. + 40 mL 0.1 mol/L HCl; mech. shaking 30 min; filtered, pH adj. to 7.0 | not given | 0.75 mL THF (DS) + 80 µL CHCl3 (ES) inj. into 5.0 mL solution + 0.5 g NaCl; centrif.; sedim. phase evaporated, rediss. in 15 µL MeOH | η 82.0%–93.4% (2 levels); RSD < 7.3%; LOD 1.0–1.6 ng/g | [78] |
DLLME | GC-FID | sediment | PAHs | SFE: 1.2 g s.s. + 50 µL MeOH (PM); SFE at T 313 K, p 253.2 bar, static textr 10 min, dynamic textr 30 min, CO2 F = 0.5 mL/min; collected in 1 mL ACN in ice bath | pressure, temperature, static & dynamic extraction time | 1.0 mL extract (DS) + 16 µL ClBz (ES) inj. into 5 mL w.; centrif.; direct injection | η 67.8%–98.9%; RSD < 10.3%; LOD 200 ng/g | [79] |
DLLME | GC-FID | soil sediment | 7 organo-phosphor. pesticides | SFE: 1.2 g s.s. . + 50 µL MeOH (PM); SFE at T 60 °C, p 150 bar, static textr 10 min, dynamic textr 30 min, CO2 F = 0.5 mL/min; collected in 1 mL ACN in ice bath | pressure, temperature, static & dynamic extraction time | 1.0 mL extract (DS) + 17 µL CCl4 (ES) inj. into 5 mL w.; centrif.; direct injection | η 80%–100%; RSD < 75%; LOD 1–9 ng/g | [80] |
DLLME | GC-FID | soil | 2 nitrotoluenes | SFE: 2 g s.s. + 150 µL MeOH (PM); SFE at T 35 °C, p 350 atm, static textr 10 min, dynamic textr 30 min, CO2 F = 0.4 mL/min; collected in 1 mL MeOH in ice bath | central composite design to optimize SFE parameters: T, pressure, VPM, dynamic textr | 1.0 mL extract (DS) + 20 µL CCl4 (ES) inj. into 5.0 mL w. (3% NaCl); centrif.; direct injection | η 80%–84%; RSD < 6.5%; LOD 0.12 µg/g | [81] |
DLLME | GC-MS | sediment | hydroxylated PAHs | SWE: 10 g s.s. + 2 g diatomaceous earth; PLE with w. pH 3.0 + 20% ACN (OM) 10 min at 150 °C & 1500 psi; purged with N2, collected 11 mL extract | type and V of organic modifier for SWE, pH, T, pressure, extr. time | 100 µL ClBz (ES) inj. into 11 mL extract (20% ACN as DS); VA 30 s; centrif.; sedim. phase evaporated, added 50 µL MTBSTFA to derivatize, evaporated, rediss. in 100 µL AC | η 57.63%–91.07%; RSD < 11.07%; LOD 0.0139–0.2334 ng/g; comparison with SWE-SPE - all parameters better for SWE-DLLME | [82] |
DLLME | GC-MS | pyrolysis solid residue | 15 aromatic volatiles | extracted s.s. (extr. with CH2Cl2) and raw s.s. leached with 0.001 M CaCl2 sol. (leach test ISO/TS 21268-2) | not given | 0.5 mL AC (DS) + 50 µL CCl4 (ES) inj. into 5.0 mL leachate; centrif.; direct injection | LOD 1.02–24.6 ng/L a; compared with static HS and HS-SPME (both lower LODs) | [83] |
DLLME | GC-MS | pyrolysis solid residue | 11 alkylphenols | extracted s.s. (extr. with CH2Cl2) and raw s.s. leached with 0.001 M CaCl2 sol. (leach test ISO/TS 21268-2) | not given | 1.0 mL AC (DS) + 15 µL TtCEt (ES) inj. into 4.0 mL leachate + NaCl (15%); centrif.; direct injection | η 61.9%–101.4%; RSD < 8.0%; LOD 0.07–0.17 µg/L b | [84] |
DLLME | GC-MS | particul. matter in seawater | 8 UV filters | unfiltered seawater, US 15 min; pH adj. to 2.5 with acetic a.; filtered | US time | 250 µL AC (DS) + 50 µL CHCl3 (ES) inj. into 5.0 mL sample; centrif.; direct injection | η 88%–117% (2 levels); RSD < 14%; LOD 10–30 ng/L a | [85] |
DLLME & in-syringe back-extract. | HPLC-UV | soil sediment | 5 chlorophenols | MWE: 1.2 g s.s. + 2 mL w. (pH 10.0); MWE 90 s, cooling, diluted to 5 mL with w., pH adj. to 6.0; centrif., filtered | Vsolv, pHsolv, MWE time | 1.0 mL AC (DS) + 37 µL ClBz (ES) inj. into 5.0 mL extract; centrif.; 20 µL sedim. phase in syringe, then 20 µL w. (pH 12.0), plunger moving 5 min; w. phase injected | η 66.1%–82.0%; RSD < 7.6%; LOD 0.5–2.0 ng/g; chromatograms free of interferences | [86] |
USA-EME | HPLC-DAD | soil | triazine herbicides | 10 g s.s. + 10 mL w.; mech. shaking 40 min; filtered, diluted to 10.0 mL with w. | not given | 5.0 mL extract + 100 µL ClBz,; US 3 min at 25 °C; centrif.; sedim. phase evaporated, rediss. in 20 µL MeOH | η 82.6%–92% (2 levels); RSD < 4.3%; LOD 0.1–0.5 ng/g | [87] |
ATPS | HPLC-UV | soil | 2 phytohormones | 10 g s.s. + 30 mL MeOH/w. (80:20); US 20 min; centrif.; repeat; filtered, evaporated, rediss. in 10 mL MeOH/w. (80:20, pH 3) | not given | 1.0 mL solution + 0.6 g [BMIM]Br + 0.75 g K2HPO4; stirred 10 min at 30 °C; centrif.; upper phase collected, direct injection | η 86%–102%; RSD < 5.3%; LOD 2–10 ng/g; compared to direct HF-LPME | [88] |
CAE-ME | HPLC-DAD | sediment | PAHs, alkyl-phenols, paraben | MWE: 0.1 g s.s. + 3 mL 40 mM CTAB solution; MWE for 6 min at 90 °C and 140 W, cooled; centrif., filtered | T, MW power, CTAB solution V and concentration | 2 mL solution + 200 µL ACN + 46 µL Li-NTf2 0.5 g/mL; VA 3 min; heated 2 min at 65 °C; centrif.; sedimented droplet dil. to 100 µL with ACN, VA | η 92.8%–95.7% (2 levels); RSD < 19.3%; LOQ 0.02–0.36 µg/g; several interferences from the sample co-extracted | [89] |
in-situ LPME with IL-based surfactant | HPLC-DAD | sediment | PAHs, alkyl-phenols, paraben | MWE: 0.1 g s.s. + 3–5 mL 40 mM C16MIm-Br sol.; MWE for 6 min at 90 °C and 140 W, cooled; centrif., filtered | T, type of ILS, ILS solution V and concentration | 4 mL solution + 800 µL ACN + 92 µL Li-NTf2 0.5 g/mL; heated 5 min at 65 °C; VA 3 min; centrif.; sedimented droplet (≈90 µL) dil. to 200 µL with ACN, VA | η (2 levels) 91.1%–127%; RSD < 19%; LOQ 0.04–1.0 µg/g | [90] |
HF-LPME; DLLME | GC-FPD | soil | 6 organosulfur pesticides | 5 g s.s. + 10 mL w.; US 40 min; centrif.; used for HF-LPME or filtered (2×), diluted 25× with w. for DLLME | not given | HF-LPME: 5.0 mL extract, 5 µL o-xylene (ES) in 1-cm HF; stirring 35 min at 1200 rpm; direct injectionDLLME: 0.8 mL MeOH (DS) + 10 µL CCl4 (ES) inj. into 5.0 mL solution; centrif.; direct injection | HF-LPME: η 81.7%–109.2%; RSD < 9.6%; DLLME: η 87.8%–100.6%; RSD < 9.0%; LOD not given for soil samples Comparison: DLLME faster & higher capacity, HF-LPME more robust & simple for complex samples | [91] |
HF-LPME | GC-MS | sediment | 12 OCPs 8 PCBs | MWE: 1 g s.s. + 10 mL w.; MWE at 600 W for 20 min at 80 °C; supernatant diluted to 10 mL | T, extraction time | 10 mL extract, 5 µL toluene (ES) in 1.3-cm HF; stirring 20 min at 700 rpm; direct injection | η 73%–111% (OCP) 86–110 % (PCB); RSD < 20%; LOD 0.07–0.70 ng/g | [92] |
HF-LLLME | LC-ESI-MS | dried sewage sludge | NSAIDs | PHWE: 0.5 g s.s. + 20 g sea sand, PLE with 0.01 M NaOH 5 min (5 cyc.) at 120 °C & 100 bar, flush V 60 %; purged with N2, collected 90 mL extract adj. pH to 1.5 and diluted to 100 mL | pH of solvent, T, number of cycles, flush volume | 100 mL extract, DHE in 10-cm HF wall (ES) & 25 µL 0.1 M (NH4)2CO3 (AS) in HF lumen; stirring 120 min at 600 rpm; direct injection | η (PHWE) 101%–109% (spike), 38.9%–90.3%(native); η (HF-LPME) 23.6%–30.3%; RSD < 20%; LOD 0.4–3.7 ng/g; only small matrix effect in ESI | [93] |
HF-LLLME | LC-ESI-MS | dried sewage sludge | SSRIs | PHWE: 0.5 g s.s. + 20 g sea sand; PLE with 0.05 M H3PO4 pH 2 for 5 min (5 cyc.) at 120 °C & 100 bar, flush V 90%; purged with N2, collected 90 mL extract adj. pH to 12.4 and diluted to 100 mL | pH of solvent, T, number of cycles, flush volume | 100 mL extract, DHE in 10-cm HF wall (ES) & 0.1 M (NH4)H2PO4 pH 2.1 (AS) in HF lumen; stirring 8 h; direct injection | η (PHWE) 67%–83%(spike) 72.2%–85.8%(native); η (HF-LPME) 29%–47%; RSD < 20.8 %; LOD 6 ng/g; comparison to direct HF-LLLME method (without PHWE) | [94] |
HF-LLLME | LC-MS/MS | sewage sludge | SSRIs and metabolites | 1 g s.s. + 1.1 L w. + 20 µL HCOOH; stirred 16 h at 900 rpm; filtered, diluted 1:100 or 1:20 | not given | solution + IS + 10 mL 5 M NaOH, DHE in 28-cm HF wall (ES) & 20 µL w.+HCOOH pH 2 (AS) in HF lumen; stirring 2 h at 800 rpm; direct injection | η 26.2%–71.4%; RSD < 24.6%(SSRI), < 51% (metab.); LOD not given | [95] |
DI-SDME | AP-MALDI-MS | soil | antibiotic monensin | 5 g s.s. + 15 mL w. (10% NaCl); shaking 5 min, US 5 min; centrif., repeat; supernatants collected | not given | 20.0 mL solution + 10% NaCl, 1.5 µL CHCl3/toluene (1:1) drop immersed for 10 min at 240 rpm; direct injection | η 74.5%–82.8% (3 levels); RSD < 6.5%; LOD 12.4 ng/mL b | [96] |
HS-SDME | GC-FID | fire debris | fire accelerants | 20x20 cm piece of textile soaked with accelerant, ignited; debris + 100 mL w., mixed 3 min; centrif., filtered | sample volume | 10 mL filtrate stirred at 1500 rpm, 2.5 µL benzyl alcohol drop exposed to HS for 20 min; direct injection | LOD 0.15 mg/L a | [97] |
ESy | GC-ECD GC-MS | soil | OCPs | 1 g s.s. + 10 mL w./ACN (8:2); US 15 min; centrif.; supernatant + 70 µL conc. H3PO4 + 100 mg Cu granules; US 15 min; filtered | ACN addition to extr. solvent | 3 mL filtrate flushed through donor side ESy at 100 µL/min; acceptor phase: n-undecane; direct injection | compared with SE and PLE: comparable results, less solvent (~4 mL vs. 420 mL-SE or 18 mL-PLE) and time (1.5 h vs. 4 h-SE or 0.85 h-PLE), less s.s. | [98] |
3.2. LPME Combined with Environmentally-Friendly Extraction
LPME | Analytical techn. | Sample | Analytes | Preparation of solid sample | LPME procedure | Optimization of extraction conditions | Method performance | Ref. |
---|---|---|---|---|---|---|---|---|
DLLME | GC-FPD | soil | chlorpyrifos | "soil solution" a | 1.5 mL MeOH (DS) + 40 µL 1-dodecanol (ES) inj. into 25 mL solution at 40 °C; kept still 5 min, added 0.5 g NaCl, shaken; centrif.; ice bath to solidify drop, rinsed with ice w., diss. in 60 µL EtAc | extraction solvent type & V, disperser solvent type & V, mass of NaCl, extr. time | η 84%–103% (2 levels); RSD < 6.4%; LOD 0.084–0.52 ng/mL b | [99] |
US-DLLME | GC-MS | house dust | TBBPA | Kimwipe sprayed with MeOH/AC (1:3), 1 min wiping of 100 cm2 area | 1 cm2 Kimwipe + 800 µL w. + 100 µL MeOH/AC (1:3, DS) + 30 µL ClBz (ES) + 1 drop HClconc + 50 µL Ac anhydride; US 5 min; centrif.; sedim. phase added Ac anhydr., IS & CH2Cl2 to 56 µL; US 5 min; heated 60 °C for 5 min, injected | disperser solv. type & V, extraction solvent type & V, swabbing material | η 104%–106%; RSD < 18%; LOD 2.5 ng/mL; compared with SPE | [100] |
HF-LPME | GC-FID | soil | 6 PAHs | 1 g s.s. + 7 mL AC + 15 mL w.; shaking 30 s | 22 mL suspension, 8 µL octane (ES) + IS in 6.5-cm HF; stirring 8 min at 1350 rpm; direct injection | extraction time; HF: stirring rate, VAC, extr. time, VES | η 2.9%–6.2% (PF 80.1–170.7); RSD < 23.3%; LOD 130–220 ng/g | [101] |
HF-LPME | HPLC-UV | soil | 2 phytohormones | none | 5 g s.s. + 14 mL NaCl sol. (340 g/L), 10 µL [BMIM]PF6 (ES) in 2.5-cm HF as solvent bar; stirring 50 min at 900 rpm and 25 °C; direct injection | Vsolv, extr. time, T, NaCl concentration, stirring rate | η 40%–60%; RSD < 7.9%; LOD 5–30 ng/g; compared to ATPS | [88] |
HF-LPME | GC-MS | soil | 8 triazines | prepared slurry: 20 g s.s./mL w., added NaCl to 10% | 3 µL toluene (ES) in 1.3-cm HF in soil slurry; extr. for 20 min at 1000 rpm | extraction solvent, extraction time, stirring rate, addition of NaCl, pH, humic acids | η not given; RSD < 5%; LOD not given; compared with SDME (drop unstable) & SPME (poorer precision) | [102] |
HF-LPME | GC-MS | soil | 4 chlorophenols | 30 mg s.s. + 15 mL w. + IS | 15 mL suspension + 15 mL pH 1 buffer sol., 15 µL 1-octanol (ES) in 5.0-cm HF, stirring 80 min at 1100 rpm; direct injection | pH & ionic strength of donor sol., stirring rate, extraction time | η 90.52%–106.47%; RSD < 5.13%; LOD not given for soil; compared with SPME - with HF-LPME less interference | [103] |
HF-LPME, dynamic | GC-MS | soil | methylphenols chloro-benzenes, chlorinated pesticides | 1 g s.s.+ 4 mL AC/w.(40:60).; US (5 min); stirring at 1000 rpm (40 min) | 4 mL suspension, 3 µL toluene (ES) in 1.3-cm HF, stirring 4 min at 200 rpm, dynamic extr. (syringe plunger); direct injection | type & ratio org. solv.: w. in suspension; HF: extr. solvent, extr. time, plunger speed, ionic strength, HA conc. | η 92%–100%; RSD < 13.0%; LOD 50–100 ng/g; comparison with SPME | [104] |
HF-LLLME | LC-ESI-MS | sewage sludge | SSRIs | 0.25–1 g s.s. + 50 mL w., pH adj. to 12.4 | 50 mL suspension, DHE in 20-cm HF wall (ES) & 10 µL 0.1 M (NH4)H2PO4 pH 2.1 (AS) in HF lumen; stirring 6 h; direct injection | pH of sample suspension, acceptor solvent & pH, extraction time | η 5%–19% (PF 221-995); RSD < 18.4%; LOD 1–12 ng/g; comparison to HF-LLLME after PHWE | [94] |
HF-LLLME | LC-ESI-MS | sewage sludge | 4 NSAIDs | 0.5–1.5 g s.s. + 50 mL w., stirred 17 h at 660 rpm, pH adj. to 1.5 | 50 mL slurry, DHE in 18-cm HF wall (ES) & 10 µL 0.1 M (NH4)2CO3 pH 9 (AS) in HF lumen; stirring 4 h at 660 rpm; direct injection | extraction time | η not given; RSD < 17.7%; LOD not given | [105] |
DHF-HS-LPME | GC-MS | soil | 6 PAHs | 1 g s.s. + 1 mL w.; heated at 90 °C for 10 min | 3 µL 1-octanol (ES) in 1.5-cm HF in headspace over soil slurry heated at 40 °C for 10 min at 400 rpm, dynamic extr. (5 s dwell time); direct injection | extraction solvent, dwell time, number of cycles, extraction time, T, addition of w. & NaCl to s.s. | η not given; RSD < 14.6%; LOD 5.9–76 ng/g | [106] |
HS-SDME | GC-FID | drilling mud | C6-C12 hydrocarbons | drilling mud with water left to separate | 5 mL supernatant in vial, a drop (1.5 µL) of n-hexadecane (ES) + IS suspended from needle tip in HS; extr. for 30 min at 1000 rpm; direct injection | extraction solvent type & V, ionic strength of sample, stirring rate, extraction time | clean chromatograms with no intereferences; other data not given for drilling mud | [107] |
HS-LPME | GC-ECD | soil | 5 chlorobenzenes | 1 g s.s. + 1.5 mL w.; heated for 30 min at 40 °C before extr. | 2 µL toluene (ES) into 10-µL microsyringe, 5 µL HS at 40 °C withdrawn at 1µL/s, expelled, 5 s waiting, repeat 25 times; direct injection | extraction solvent type & V, HS sampling volume, withdrawal rate, number of cycles | η not given; RSD < 17.7%; LOD 6–14 ng/g; compared with HS-SPME | [44] |
CF-SDME (GF-HS-LPME c) | GC-MS | sediment | PAHs | not given | continuous gas flow SDME in a home-designed apparatus: sample heated at 80 °C, extr. for 20 min into 2 µL dodecane (ES) in the gas channel, gas flow rate 2.7 mL/min | gas flow rate, position of solvent drop, i.d. gas outlet channel, extraction time, sample T, extr. solvent T | η not given; RSD < 19.7%; LOD 0.020–8.0 ng d | [108] |
4. LPME without Previous Extraction of Solid or Semisolid Samples
5. Conclusions
Acknowledgments
Conflicts of Interest
References
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Prosen, H. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples. Molecules 2014, 19, 6776-6808. https://doi.org/10.3390/molecules19056776
Prosen H. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples. Molecules. 2014; 19(5):6776-6808. https://doi.org/10.3390/molecules19056776
Chicago/Turabian StyleProsen, Helena. 2014. "Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples" Molecules 19, no. 5: 6776-6808. https://doi.org/10.3390/molecules19056776