membranes

Review
Environmental Applications of Electromembrane Extraction:
A Review
Linping Shi 1,2 , Mantang Chen 2, * , Ge Zhao 2 , Xiaoyu Wang 2 , Meijuan Fan 2 , Ruihong Liu 2 and Fuwei Xie 2, *

1 College of Chemistry, Zhengzhou University, Science Avenue #100, Zhengzhou 450001, China;
[email protected]
2 Zhengzhou Tobacco Research Institute of CNTC, Fengyang Street #2, Zhengzhou 450001, China;
[email protected] (G.Z.); [email protected] (X.W.); [email protected] (M.F.);
[email protected] (R.L.)
* Correspondence: [email protected] (M.C.); [email protected] (F.X.); Tel.: +86-0371-67672396 (M.C.);
+86-0371-67672502 (F.X.)

Abstract: Electromembrane extraction (EME) is a miniaturized extraction technique that has been
widely used in recent years for the analysis and removal of pollutants in the environment. It is based
on electrokinetic migration across a supported liquid membrane (SLM) under the influence of an
external electrical field between two aqueous compartments. Based on the features of the SLM and
the electrical field, EME offers quick extraction, effective sample clean-up, and good selectivity, and
limits the amount of organic solvent used per sample to a few microliters. In this paper, the basic
devices (membrane materials and types of organic solvents) and influencing factors of EME are first
introduced, and the applications of EME in the analysis and removal of environmental inorganic ions
and organic pollutants are systematically reviewed. An outlook on the future development of EME
for environmental applications is also given.

Keywords: electromembrane extraction; environmental analysis; environmental remediation; inor-

ganic ions; organic pollutants

Citation: Shi, L.; Chen, M.; Zhao, G.;

Wang, X.; Fan, M.; Liu, R.; Xie, F.
1. Introduction
Environmental Applications of
Electromembrane Extraction: A Serious environmental pollution has attracted increasing attention because of its
Review. Membranes 2023, 13, 705. toxicity and bioaccumulation. It is highly challenging to accurately identify environmental
https://doi.org/10.3390/ pollutants, especially at trace levels, without pre-treatment procedures. The most popular
membranes13080705 technique for completely extracting organic chemicals from solid samples is called soxhlet
extraction, and it was created in 1879. However, there are several drawbacks to Soxhlet
Academic Editor: Stanislav
extraction, including the length of time needed (usually 16 to 24 h) and the amount of
S. Melnikov
solvent required (often 100 to 500 mL). Pressurized liquid extraction (PLE) was introduced
Received: 19 June 2023 in 1996 as an alternate extraction method and had the advantage of decreased extraction
Revised: 24 July 2023 time. However, when using a nonpolar extraction solvent, wet samples must be dried
Accepted: 27 July 2023 before analysis, which is a disadvantage of PLE for all classes of analytes [1]. Researchers
Published: 28 July 2023 have been compelled to develop novel, effective, economical, environmentally friendly,
and secure extraction procedures as a result of these limitations.
Liquid-phase microextraction techniques (LPME) use a liquid medium (ionic liquids,
single organic solvents, or mixed organic solvents) as the extraction phase. To begin,
Copyright: © 2023 by the authors.
100 µL or less of solvent is loaded in a support, such as hollow fiber (HF) or membrane, by
Licensee MDPI, Basel, Switzerland.
specific techniques (coating or impregnation). Liquid-phase microextraction techniques
This article is an open access article
distributed under the terms and
allow the separation and enrichment of trace targets from complex matrices. Zhao and
conditions of the Creative Commons
Lee [2] presented the HF-LPME in 2002 to address the shortcomings of LPME, including
Attribution (CC BY) license (https://
unstable droplets, easy to fall off from the tip of the needle, and poor repeatability. In HF-
creativecommons.org/licenses/by/ LPME, target analytes are extracted from aqueous samples and transferred to a supported
4.0/). liquid membrane (SLM) maintained in the pores in the wall of a small porous hollow

Membranes 2023, 13, 705. https://doi.org/10.3390/membranes13080705 https://www.mdpi.com/journal/membranes

Membranes 2023, 13, 705 2 of 17

fiber, then to an acceptor phase inside the hollow fiber’s lumen. The main benefits of
these techniques are their low cost, ease of use, small sample volume, rapidity, extremely
low solvent consumption, high enrichment factor, and reduced waste generation. The
electromembrane extraction (EME) proposed by Pedersen-Bjergaard and Rasmussen in
2006 further improved the extraction efficiency and extraction time on this basis [3].
The classical EME device applies an electric field at two electrodes in the sample
solution and the hollow fiber lumen based on the HF-LPME device [4]. Another type
of EME device is the two-phase EME. A plastic centrifuge tube (2 mL) was used as the
donor chamber and a 1000 µL pipette tip as the acceptor chamber, with a polypropylene
membrane sealed at the bottom of the tip. Two platinum electrodes were embedded in the
donor and acceptor with an average distance of 1 cm between the electrodes [5]. In EME,
charged analytes are extracted from the aqueous sample solution across an SLM and into an
aqueous acceptor phase while being subjected to an electrical field. The acceptor phase was
then collected for chemical analysis. The SLM is a porous polymeric support membrane
that has an organic solvent immobilized by capillary forces. The use of nanostructured
materials, biopolymer membranes, and gels as supporting liquid membranes has also
been reported. SLM is selective for the extraction of target analytes and therefore provides
excellent sample clean-up capability [6]. An electrical potential (DC) sustained over the
SLM, with one electrode positioned in the sample and the other electrode positioned in
the acceptor phase, serves as the driving force for the extraction [3]. The pH of the sample
and the acceptor solution must both be neutral or acidic to preserve the protonated state of
the cationic analytes (basic chemicals) during extraction. The target analytes are therefore
vulnerable to electrokinetic migration because they are positively charged species. The
anode is in the sample, while the cathode is in the acceptor solution. For extraction of
anionic analytes (acid substances), the pH in the sample and the acceptor solution is neutral
or alkaline to maintain the analytes negatively charged. Thus, the electric field is in the
opposite direction.
Most articles focus on the analysis of inorganic ions and organic pollutants in the
environment. A few articles explore the application of EME in environmental remediation.
In this review, we present an overview of the application of EME in the environment in
recent years. Finally, critical insights into the future trends of EME are provided.

2. Basic Experimental Equipment and Parameters

The standard instrumental setup is a modification of the HF-EME device. The sample
vial is pipetted with donor solution and set on an agitator. In order to create the SLM,
the HF extraction unit is briefly impregnated with the proper organic solvent, and the HF
lumen is then filled with the acceptor solution. The HF is added to the donor solution, the
electrodes are inserted with one electrode in the donor solution and the other in the acceptor
solution, and the electric potential is turned on. To achieve effective analyte replenishment
at the donor/SLM phase contact, which is crucial for high extraction recovery and fast
extraction speed, agitation of operational solutions is preferable. In the actual example,
basic analytes quickly reach the SLM/acceptor phase contact by migrating into and across
the SLM as charged species. Utilizing an acidic acceptor phase (such as diluted acid or an
acidic buffer) allows the analytes to be released into the acceptor solution while maintaining
their protonated state. Analytes can be gradually preconcentrated in the acceptor solution
thanks to the protonation of basic analytes, which prevents their back-extraction into SLM.
Due to their respective lack of positive charges, neutral and acidic matrix chemicals do not
participate in the EME process, and even if they were to diffuse into the SLM, they would
not significantly liberate any acidic acceptor solution. After the extraction is finished, the
acceptor solution is collected and put into a vial for analysis using high-performance liquid
chromatography (HPLC), gas chromatography (GC), capillary electrophoresis (CE), etc.
Success in EME depends heavily on the mass transfer of the SLM [7]. The standards
for quality SLM candidates include (a) high polarity-polarizability, (b) low vapor pressure,
(c) high affinities and robust chemical interactions between the analyte and the organic
Membranes 2023, 13, 705 3 of 17

solvent, and (d) low water solubility [8]. Researchers have experimented with many meth-
ods to increase the mass transfer through the SLM in EME. Hasheminasab and Fakhari [9]
decorated hollow fibers (HF) with carbon nanotubes (CNTs) and thus increased the overall
analyte partition coefficient over the SLM. Huang et al. [10] discovered that the SLM vol-
ume was crucial for stable EME and that raising the SLM volume (thickness) might lower
the extraction current during EME.
The most frequently used and effective solvent in EME for nonpolar (log P > 2) basic
drugs has been 2-nitrophenyl octyl ether (NPOE). For protonated basic compounds (log
P > 2), hydrogen bond interactions have been proposed as the primary mechanism of
solvation. Recently, several NPOE substitutes have been proposed. HosseinyDavarani
et al. [11] selected 2-ethyl hexanol as a solvent for SLM, and the study showed that the
recovery was up to 85%. Drouin et al. [12] investigated 22 organic solvents as novel loading
liquid membranes and showed that 2-nitrophenyl pentyl ether (NPPE) extracted polar
metabolites with the highest efficiency, high extraction yield (EY) and reproducibility, and
with large coverage of the extracted metabolites. The optimized experimental parameters
were successfully used for the extraction of precipitated plasma samples. Pure NPOE is
ineffective for more polar basic chemicals (log P < 2) as mass transfer from the sample
and into the SLM is inefficient. An ion pair reagent, such as di-(2-ethylhexyl) phosphate
(DEHP) or tris-(2-ethylhexyl) phosphate (TEHP), was added to the organic solvent to
produce ion pairs with the analytes to improve the transport of polar drugs through SLM.
However, the current in the system is increased by the addition of DEHP. Tributyl phosphate
(TBP) and di(2-ethylhexyl) phosphite hydrogen salts are used as substitutes for the polar
basic analytes in EME. Effective SLM solvents have high hydrogen-bond basicity (very
high Kamlet–Taft β-value), high polaritypolarizability (high Kamlet–Taft π*-values), no
hydrogen-bond acidity (zero Kamlet–Taft α-values) and contain alkyl groups equivalent
to 12–18 carbon atoms [13]. For the extraction of acidic medicines, NPOE is ineffective as
the SLM. Strong hydrogen bond acidity in the SLM solvent is necessary for the EME of
acidic materials, and typical SLMs are made of aliphatic alcohols such as 1-octanol and
1-heptanol. Aliphatic alcohols are insoluble in water and tend to impregnate films.
Polypropylene (PP) is often chosen as the material used in EME procedures [14]. How-
ever, this material is plastic and disposable, and is harmful to the environment. Therefore,
these drawbacks have been overcome by modifying the liquid membrane or commercial
support. Some additives such as carrier agents, nanoparticles (NPs), and molecularly
imprinted polymers (MIPs) are usually added to change the chemical composition of
SLMs [15,16]. In addition, the use of agarose gels instead of conventional polymeric porous
membranes in EME and without the use of organic solvents has also been reported [17].
Agarose is considered to be a green material. Another recent development in EME environ-
mental applications is the application of green biodegradable membranes instead of classic
SLMs. Materials derived from biopolymers (such as agarose or chitosan) are biodegradable
and sustainable materials and have recently gained a lot of attention in EME [14,17,18].
These materials, which are obtained from natural resources, are environmentally friendly,
and have low economic costs.
Huang et al. [19] proposed a time-dependent transient model to simulate the mass
transfer of SLM in EME. This model is mostly based on three hypotheses: (a) the SLM
residence time of the analyte produces a lag time, (b) the transport via the SLM is the
extraction stage that determines the rate, and (c) there is only one direction of transport
through the SLM [20]. This model confirms that the voltage applied across the liquid
membrane is the main operating parameter in EME. The voltage is typically provided
between 5 and 600 V. Recovery values decline at higher voltages due to electrode bubble
formation and system instability [3]. Time is another important parameter that affects
recovery. There are several possibilities for the decrease in recovery over time: (a) unstable
current in the system, (b) elevated pH in the acceptor phase, (c) diffusion of analytes into
the donor phase, and (d) loss of a small amount of artificial liquid film [20]. Typically, the
extraction process takes no longer than 15 min.
Membranes 2023, 13, 705 4 of 17

During EME, pH can shift in both the sample and the acceptor phases. It has been
shown that a decrease in the ratio of total ion concentration on the donor side to total
ion concentration on the recipient side increases ion flux [21]. The analytes are extracted
across the SLM in EME, with a positive electrode placed in the sample and a negative
electrode placed in the acceptor solution to quickly extract basic analytes. The pH in the
sample and acceptor solutions must be low to ionize the analytes. The pH of the donor and
acceptor solutions was alkaline during the extraction of acidic drugs. Acceptor solutions
with high concentrations of weak organic and strong mineral acids can produce stable EME
performance [22].
Stirring speed increases mass transfer and decreases the thickness of the bilayer around
the SLM, improving extraction kinetics and extraction efficiency [23]. The donor solution
is typically vigorously stirred or agitated to ensure an efficient, long-lasting interaction
between the analyte ions and the SLM surface. Typically, stirring is maintained at a speed
of 0–1250 rpm [23]. Due to the production of bubbles in the donor and acceptor phases, as
well as the leaking of the organic solvent from the SLM, extraction recovery is reduced at
higher stirring rates.
Basically, the diffusion coefficient also increases with increasing temperature, but
the driving force of the system decreases with increasing temperature [21]. To assess the
impact of sample solution temperature, Rahmani et al. [24] used a range of sample solution
temperatures (25–60 ◦ C) during the extraction process while monitoring the extraction
recovery and membrane current intensity. The results suggest that when the temperature of
the donor solution rises, extraction recovery follows a declining pattern. Temperatures up
to 40 ◦ C can hasten the extraction process, while those above 40 ◦ C can partially degrade
the SLM [25].

3. EME for Environmental Analysis

Environmental analysis refers to the process of measuring the possible pollutants and
sources of pollution in an environment using specific technical means, which can provide
accurate and critical reference information and a basis for environmental protection work.
EME is a common pretreatment method for environmental samples with complex matrices
that cannot be directly detected by analytical instruments. Most references in this review
use water samples as an example to explore the feasibility of EME in the environmental
analysis.

3.1. Determination of Inorganic Ions by EME

Inorganic ionic pollutants, including dichromate, perchlorate, and heavy metal cations,
are pervasive in the environment and pose substantial risks to people and the natural
world. For example, when inhaled or placed in contact with skin, Cr(VI) damages the
kidney and liver and is more difficult to treat than other pollutants that decompose through
enrichment [26]. Arsenate is a highly biotoxic substance that can lead to poor nutritional
growth in plants, and the introduction of arsenate into the human body alters the normal
metabolism of cells [27].
Tan et al. [28] designed and fabricated a concentric electromembrane extraction pre-
concentration device for the determination of NO3− and SO24− content from a soil slurry
without additional treatment using fused deposition modeling 3D printing technique. A
smaller, hemispherical 3D-printed porous membrane acceptor vial was placed within the
larger, hemispherical electrode sample vial made of conductive polylactic acid filament.
The system is efficient at ion extraction from numerous samples into a smaller acceptor
solution. Fluorescein was used to image the extraction process in order to demonstrate
electromembrane extraction, with preconcentration rates of 8.33 × 10−7 mol/L per second
at 120 V and close to 95% recovery. The enrichment factor was between 36–44 and the LOD
was between 1.6 × 10−7 –1.8 × 10−7 mol/L. The NO3− and SO24− concentrations extracted
and quantified from the soil slurry were within the range of values typically reported in
Membranes 2023, 13, 705 5 of 17

soil samples. For strong acid anions, the device showed good recovery, but it performed
poorly for weak acid anions.
Khan et al. [29] reported the effective EME of Cu(II) in different environmental water
samples followed by Red-Green-Blue (RGB) detection. The applied voltage, the extraction
time, the composition of the SLM, the pH of the acceptor/donor phases, and the stirring
rate are the effective parameters that have been optimized for the extraction efficiency of
EME. 1-octanol was adopted as the SLM and 0.1 mol/L HCl was used as the donor and
acceptor solutions. A voltage of 50 V was used as the driving force, the system was agitated
at 400 rpm, and the extraction time was 15 min. The relative recoveries were in the range
of 93–106%. The enrichment factor was 100. The method provides a rapid, simple, and
effective determination of Cu(II).
Nojavan et al. [30] discussed the use of free liquid membranes (FLM) for the micro-
electromembrane extraction (µ-EME) of Cr(VI) from wastewater samples. Electrothermal
atomic absorption spectrometry was used to calculate the amount of Cr(VI). It was opti-
mized for FLM and acceptor solution types, donor and acceptor solution pH, electrical
potential, and FLM thickness. The SLM was composed of 1-octanol containing 5% methyl
trialkyl-ammonium chloride with a thickness of 1 mm, and the extraction time was 5 min.
In addition, 0.5 mol/L NaClO4 and 0.1 mol/L HCl were used as the acceptor and donor
phases, respectively. The driving force for the extraction was 75 V. According to the conven-
tional addition approach, relative recoveries of the spiked Cr(VI) in the samples ranged
from 73.8 to 85.1%. The calculated limit of detection was less than 0.06 ng/mL. µ-EME is a
promising option for the selective extraction of Cr(VI).
Kaya [31] made improvements to the membrane process to improve the long-term
use and stability of the membrane. Amine functional reduced graphene oxide (rGO-fNH2 )
and modified membrane including 51.85% NPOE, 29.63% cellulose triacetate, and 18.52%
rGO-fNH2 were synthesized. In an experiment with the constant current instead of constant
voltage, the membrane stability was still above 90% after 30 repetitions. Improvements
made to the membrane process have improved the long-term use and stability of the mem-
brane. However, the use of electricity during the experiments can damage the membrane
structure.
Tabani et al. [32] chose positively charged Cr(III) and negatively charged Cr(VI) as
model analytes, and investigated the effect of electroendotropic (EEO) flow phenomenon on
gel electroemulsion extraction (G-EME). A low-cost, simple-to-use reading platform known
as a microfluidic paper-based analytical device was used to quantify both compounds.
By using G-EME for the determination of chromium in water samples, the instrument
has a high level of environmental friendliness, improved sensitivity, and higher analytical
performance by enrichment extraction. The recoveries were 87% for Cr(III) and 75%
for Cr(VI). The LODs were 0.5 and 0.7 ng/mL for trivalent and hexavalent chromium,
respectively.
Fashi et al. [33] reported the EME combined with microvolume UV-Vis spectrophoto-
metric detection of mercury in water and fish samples. For the electromembrane extraction
of mercury, 1-octanol and 2% (v/v) DEHP was chosen as the appropriate membrane com-
position. The pH of the donor solution (0.01 mol/L NaOH) was 7.0 and the pH of the
acceptor solution (0.01 mol/L NaOH) was 3.0. The driving force for the extraction was
12 V, and the unit was agitated at 700 rpm for 10 min. The LOD was found to be 0.7 µg/L
and 12 µg/kg in water and fish samples, respectively. The repeatability and reproducibility
of the procedure were excellent.
Silva et al. [34] reported the simultaneous EME of six trace metal cations (Cu2+ ,
Zn ,Co2+ , Ni2+ , Pb2+ , Cd2+ ) from saline samples. Metals in acceptor solutions were
2+

identified using CE with capacitively linked contactless conductivity detection (C4 D). The
SLM was composed of 1-nonanol containing 1% (v/v) di-2-ethylhexyl phosphoric acid
(DEHPA). The driving force was 10 V, and the extraction time was 20 min. The extraction
unit was stirred with a stirring rate of 750 rpm. The pH of the donor solution was 5.0 and
the acceptor solution was 1 mol/L acetic acid. The approach demonstrated high linearity in
Membranes 2023, 13, 705 6 of 17

the concentration range of 5 × 10−7 –10−6 mol/L and reproducibility between 8 and 21.8%
(n = 5). The LOD of this method is better than 2.6 × 10−9 mol/L.
Table 1 summarizes the applications of EME in the determination of inorganic ions.

Table 1. Applications of EME for determination of inorganic ions.

Enrichment Factor
Matrix Analyte SLM Composition Detection System Voltage (V) and/or Recovery LOD Ref.
EF Recovery
Wastewater
1-octanol containing
samples, a nano Heavy metal
0.5% DEHP and 0.5% AAS 60 - >71.2% - [35]
silver suspension cations
TEHP
sample
Drinking water
0.25–0.35
and environmental Perchlorate 1-heptanol CE-C4 D 25 - 95.9–106.7% [36]
µg/L
samples
NPOE containing 1% Fluorescence
Water Uranium (VI) 80 >64.7 >54% 0.1 ng/mL [37]
DEHPA measurements
Drinking water 1-pentanol and
Perchlorate CE-C4 D 150 30 - - [38]
samples 1-hexanol
Digital
NPOE containing 15%
Water samples Cr(VI) image-based 70 - - 10 µg/L [39]
DEHP
colorimetry
Water samples Cr(VI) 1-octanol ETAAS 15 106 - 0.06 ng/mL [40]
Water samples Hg(II) 1-octanol SWASV 60 - 89–97% 0.01 µg/L [41]
Food supplement Iodide: 18
Iodide and Portable
and drinking water Gel 50 - - µg/L; Cr(VI): [42]
Cr(VI) spectrometer
samples 5 µg/L
Wastewater sample Basic drugs 3% of agarose gel HPLC/UV 25 - - 1.5–1.8 ng/mL [43]
Cr(VI) and
Water samples 1-octanol HPLC 30 - 31.1–47.2% 5.4 µg/L [44]
Cr(III)
Cr(VI): 2.0
Cr(III) and Cr(VI): 58.8%;
Water samples Agarose gel µPADs 65 ng/Ml; Cr(III): [17]
Cr(VI) Cr(III): 83.3%
3.0 ng/mL
1-octanol with 2.5%
Water samples As(III) ASV 70 - - 0.18 mg/L [45]
DEHP
Water samples Cr(VI) 2-NPOE UV-Vis 10–50 - 54.73% - [46]
Tap water and river 1-octanol with 102–
Hg(II) GFAAS 60 41–43% 0.5 µg/L [47]
water sample 2.0% DEHP 108
Cr(VI): Octanol-1;
Drinking water Cr(VI): 0.7
Cr(III) and Cr(III): DEHP
and mineral water µPADs 70 - - µg/L; Cr(III): [48]
Cr(VI) containing octanol-1
samples 1.0 µg/L
(0.7%)
Tap water and 1-octanol containing
Heavy metal 2.5 × 10−8 –2
powdered milk 0.5% bis(2-ethylhexyl) CE-C4 D 75 - - [49]
cations × 10−7 mol/L
samples phosphonic acid
Pure water samples
Inorganic 67–
and water miscible 1-heptanol Ic 15 - 0.6–7.5 ng/mL [50]
anions 17
organic solvents
1-octanol containing
Water samples As(V) UV-Vis 70 - 95–102% 1.5 ng/mL [51]
2.5% DEHP
Tap water, river
Cr(VI) and
water, and mineral 2-ethyl hexanol ET-AAS 300 110 66 0.02 ng/mL [52]
Cr(III)
water samples
Mineral water,
drinking water, tap
Cr(VI) NPOE UV-Vis 100 80 95–125% - [53]
water, and surface
water
Nitrobenzene
Sea water Bromide containing 3% (w/w) CE-C4 D 25 - - - [54]
BU6
Tap, river and 20% DEHPA in 9 × 10−11
Pb(II) SWV 5 - 80.0% [55]
seawater 1-octanol mol/L
Membranes 2023, 13, 705 7 of 17

Table 1. Cont.

Enrichment Factor
Matrix Analyte SLM Composition Detection System Voltage (V) and/or Recovery LOD Ref.
EF Recovery
1-octanol containing 5%
Water samples thorium UV-Vis 90 50 - 0.29 ng/mL [56]
DEHP
dPKBH dissolved in
Natural waters Copper ions AAS 95 - - 0.004 mg/L [57]
1-nonanol
NOPE containing 15.0%
Spring water Copper ions µPADs 30 - - 20.0 µg/L [58]
DEHP and 5.0% TEHP
Water samples Zn(II) Gel FAAS 50 - - 5.0 µg/L [59]
Water and food
Lead 1-octanol GFAAS 30 111 86.7–116.0% 0.011 ng/mL [60]
samples
Seawater Nickel DEHPA GFAAS 25 180 - 23.3 ng/L [61]
Tap water, food,
Copper ions 1-octanol RGB 10 - - 0.1 µg/mL [62]
and soil samples
Wastewater sample Lead 1-octanol RGB 9 - 97–102.6% - [63]
Note: Atomic absorption spectroscopy (AAS); Capillary electrophoresis with capacitively coupled contactless
conductivity detection [CE-C4 D]; Electrothermal atomic absorption spectrometry (ETAAS); Square wave an-
odic stripping voltammetry (SWASV); polyaniline (PANI); Gold nanoparticle-modified glassy carbon electrode
(AuNP/GCE); High performance liquid chromatography (HPLC); Microfluidic paper-based analytical devices
(µPADs); Anodic stripping voltammetry (ASV); Di-(2-ethylhexyl) phosphate (DEHP); di-2-ethylhexyl phosphoric
acid (DEHPA); Electrothermal atomic absorption spectrometry (ET-AAS); Di-2-pyridyl ketone benzoylhydrazone
(dPKBH); Ultra high resolution mass spectrometry (UHRMS); Diode array detection (DAD); Graphite furnace
atomic absorption spectrometry (GFAAS); Electrospray ionization (ESI); Fluorescence detection (FLD); Flame
ionization detection (FID); Ion chromatography (IC); Bambus[6]uril (BU6); Square wave voltammetry (SWV);
Tandem mass spectrometry (MS-MS); Ultra-performance liquid chromatography (UPLC); Limit of detection
(LOD); Enrichment factors (EF); “-” It means that the cited article does not mention or does not contain this item.

3.2. Determination of Organic Pollutants by EME

Organic pollutants including cationic quaternary ammonium salts, anionic dyes,
phenolics, drugs, and additives are highly toxic, mutagenic, carcinogenic and difficult to
degrade. The direct discharge of untreated pollutants into water bodies affects the growth
of plants and animals and human health.
Mollahosseini et al. [5] reported a novel flat plate membrane for extracting DEHP
from the aqueous phase using a two-phase EME technique. The electrospinning tech-
nique was adopted to create polyacrylonitrile (PAN)/polydimethylsiloxane (PDMS) and
PAN/PDMS/titanium dioxide (TiO2 ) membranes. When the electrospun nanofibers con-
tained 3.3% (w/v) TiO2 nanoparticles, the extraction efficiency was best. After increasing
the TiO2 nanoparticle concentration to 4.4% (w/v), the TiO2 nanoparticles aggregated in-
side the nanofibers and formed beads, which would reduce the specific surface area of the
electrospun nanofibers and lead to a decrease in the performance of the membrane. The
extraction time was 20 min, and the donor pH was 5.0. A small volume of 1-octanol (0.8 mL)
was used as the acceptor solution. DEHP was detected by UV-Vis spectrophotometry. In the
concentration range of 20–1000 ng/mL, the relative standard deviation (RSD), the limit of
detection (LOD), and the limit of quantitation (LOQ) were 8%, 5 ng/mL, and 16.67 ng/mL,
respectively. Application on an industrial scale of the suggested technique is possible.
Guo et al. [64] used double surfactants-assisted electromembrane extraction by Tween®
20 and alkylated phosphate for the determination of cyromazine and melamine in surface
water, soil, and cucumber. To begin, 6 × 10−4 mol/L Tween® 20 and alkylated phosphate
were added to the donor phase and the SLM, respectively. Capillary electrophoresis with
capacitively coupled contactless conductivity detection was used to directly assess the
extract. The SLM was composed of 80% NPOE, 10% DEHP, and 10% TEHP. The pH of
donor solution and acceptor solution were 5.5 and 3.0, respectively. The extraction process
took 20 min with a stirring speed of 1000 rpm and an extraction voltage of 60 V. The average
recoveries ranged from 93.3 to 112%.
Rezaei et al. [65] reported a dual gel EME of model basic and acidic dyes from a
wastewater sample. The extracts did not require organic solvents and the membrane
Membranes 2023, 13, 705 8 of 17

components are highly degradable. The device was completed with green analytical
chemistry technology standards. The positively charged brilliant green (BG) and negatively
charged reactive red (RR) moved selectively from a 7.0 mL aqueous sample (pH 7.0) to the
500 µL cathodic (pH 4.0) and 500 µL anodic (pH 9.0) aqueous acceptor phases. The driving
force was 50 V, and the extraction time was 20 min. Under ideal circumstances, the LODs
were 0.020 and 0.025 ng/mL, and the extraction recoveries were 75–78% and 67–71% for
BG and RR, respectively. For both model analytes, linearity was found to be between 0.06
and 1.0 g/mL with a correlation coefficient above 0.996.
Balchen et al. [66] reported the EME of 37 different peptides from a 500 µL aqueous
sample. The extractability of peptides was linked to the highly variable physical-chemical
properties of peptides by three different SLMs. SLMs with different organic solvents (pure
eugenol, 1-octanol/di-isobutylketone/DEHP, 1-octanol/15-crown-5 ether) were tested.
This research has shown that a variety of peptides can be successfully extracted with EME
under various conditions.
HosseinyDavarani et al. [11] used a virtual rotating SLM for EME of model analytes
from wastewater and human urine samples. Unique electrode assemblies that included
a core electrode submerged inside the lumen of the SLM and five counter electrodes
encircling the SLM were used to achieve the virtual (nonmechanical) rotating of the SLM.
The electrical potential was distributed among five counter electrodes in a revolving pattern
using a specific electronic circuit. 2-ethyl hexanol was used as the SLM. The driving force
for the extraction was 200 V and the extraction time was 15 min. The RSDs ranged from
12.6 to 14.8%, and recoveries ranged from 38 to 85%.
Asadi et al. [67] prepared polyacrylamide gels as a novel membrane in EME for the
extraction of three model essential drugs (pseudoephedrine, lidocaine, and propranolol) by
HPLC-UV. A polyacrylamide gel membrane with a 2 mm thickness and a pH of 1.5 was
created. It contains 3.0% (w/w) bisacrylamide and 12.0% (w/v) acrylamide. The pH of the
donor phase was 7.0 and the acceptor phase was 4.0. The driving force for the extraction
was 85 V and the extraction time was 28 min. The ranges of the limits of quantification and
detection were 1.0–20.0 ng/mL and 0.3–6.0 ng/mL.
Table 2 summarizes the applications of EME in the determination of organic pollutants.

Table 2. Applications of EME for determination of organic pollutants.

Enrichment Factor and/or

Matrix Analyte SLM Composition Detection System Voltage (V) Recovery LOD Ref.
EF Recovery
Cationic
quaternary Anionic carrier:
ammonium di-(2-
River water
and anionic ethylhexyl)phosphoric CE-C4 D 3000 152–185 99.1–100% 0.3–0.4 µg/L [68]
samples
chlorophenoxy acid; cationic
acetic acid carrier: aliquat® 336
herbicides
River and tap
Antidepressants [C6 MIM] [PF6 ] HPLC-UV 10 110–150 88.2–111.4% 0.1–0.4 µg/L [69]
water samples
Dicamba and
Water samples 1-octanol CE 30 - - 6.03 ng/mL [70]
2,4-DB
River Phenoxy acid
1-octanol CE 7 - - 10–15 ng/mL [71]
water samples herbicides
Haloacetic
Wastewater acids and 0.072–40.3
Toluene HPLC-UV 200 - 87–106% [72]
samples aromatic ng/L
acetic acids
Wastewater, urine,
breast milk and
Acidic drugs 1-octanol CE-UV 5 - 90–94% 1–3 ng/mL [73]
spiked plasma
samples
Membranes 2023, 13, 705 9 of 17

Table 2. Cont.

Enrichment Factor and/or

Matrix Analyte SLM Composition Detection System Voltage (V) Recovery LOD Ref.
EF Recovery
Surface
0.98–1.43
environmental Parabens 1-octanol HPLC-DAD 30 30–49 - [74]
µg/L
waters
carbendazim:
Carbendazim:
Carbendazim 26;
Tap and river water 1-ethyl-2- 2.3 µg/L
and CE 300 thiaben- - [75]
samples nitrobenzene Thiabendazole:
thiabendazole dazole:
1.1 µg/L
50
Imipramine,
desipramine,
Water samples 1-heptanol GC-MS 60 - - <0.25 ng/mL [76]
citalopram
and sertraline
Basic
degradation
products of 20% (w/w) DEHP
Water samples UHPLC 100 - 15.7–99.7% 2–50 ng/mL [77]
nitrogen in NPOE
mustard and
VX
Five priority
0.17–0.61
Drinking water haloacetic 1-octanol CZE-C4 D 50 430–671 - [78]
ng/mL
acids
Cyproheptadine:
Water, urine, and Cyproheptadine Polypyrrole and <0.7 ng/mL;
GC-FID 120 - 26.8–46.9% [79]
plasma samples and ketotifen manganese dioxide Ketotifen: <1.1
ng/mL
Wastewater,
plasma, and urine Naproxen 1-octanol HPLC-UV 20 - 66% 0.3 µg/L [80]
samples
Verapamil,
Wastewater and haloperidol,
2-ethyl hexanol LC-UV 170 - - 2.0–3.0 ng/mL [81]
urine samples and
rivastigmine
Wastewater, Alfentanil,
plasma, breast milk, sufentanil and 1-octanol GC 80 - 70.5–95.2% 0.6–1.5 ng/mL [82]
and urine samples methadone
Pure water, human
Acidic drugs:
plasma,
Acidic and 1-octanol; basic 0.3–1.5
wastewater, and LC-UV 175 - 38.1–68% [83]
basic drugs drugs: 2-ethyle ng/mL;
breast milk
hexanol
samples
Alarelin,
Wastewater and leuprolide, 95% of 1-octanol
HPLC-UV 20 82–118 49–71% 0.2 ng/mL [84]
plasma samples buserelin, and and 5% DEHP
triptorelin
Water samples,
biological fluids,
Thebaine NPOE HPLC-UV 300 90–110 45–55% 15 µg/L [7]
poppy capsules,
and narcotic drugs
Wastewater,
Amlodipine,
human plasma,
verapamil and 2-ethyl hexanol HPLC-UV 300 - 36.3–88.7% - [85]
and human urine
clomipramine
samples
Seawater samples Chlorophenols 1-octanol HPLC-UV 10 23 74% 0.1 ng/mL [86]
Environmental
Chlorophenols 1-octanol GC-MS 50 2198 <0.005 µg/L [87]
water samples
Erythrosine
NPOE +5%DEHP
Water samples and crystal RGB 50 - ≥94% - [88]
and 1-octanol
violet
Produced Naphthenic 0.10–0.13
Decanol UHRMS 200 - - [89]
water acids µg/mL
Wastewater β-lactam
1-octanol MEKC-UV 300 7.6–11.5 - 18 ng/mL [90]
samples antibiotics
Membranes 2023, 13, 705 10 of 17

Table 2. Cont.

Enrichment Factor and/or

Matrix Analyte SLM Composition Detection System Voltage (V) Recovery LOD Ref.
EF Recovery
Wastewater
Cocaine NPOE CZE 100 - 89% 2.12 ng/mL; [91]
samples
Aqueous and Five basic
NPOE LC-MS 75 - 75–87% 0.4 ng/mL [92]
blood samples drugs
Note: Atomic absorption spectroscopy (AAS); Capillary electrophoresis with capacitively coupled contactless
conductivity detection (CE-C4 D); CZE with capacitively coupled contactless conductivity detection (CZE-C4 D);
Micellar electrokinetic chromatography with ultraviolet detection (MEKC-UV); 1-hexyl-3-methylimidazolium
hexafluorophosphate ([C6MIM] [PF6]); molecularly imprinted polymer-coated multiwalled carbon nanotubes
(MIP-MWCNTs); Electrothermal atomic absorption spectrometry (ETAAS); Square wave anodic stripping voltam-
metry (SWASV); polyaniline (PANI); Gold nanoparticle-modified glassy carbon electrode (AuNP/GCE); High
performance liquid chromatography (HPLC); Microfluidic paper-based analytical devices (µPADs); Anodic strip-
ping voltammetry (ASV); Di-(2-ethylhexyl) phosphate (DEHP); Electrothermal atomic absorption spectrometry
(ET-AAS); Diode array detection (DAD); Graphite furnace atomic absorption spectrometry (GFAAS); Electrospray
ionization (ESI); Fluorescence detection (FLD);“-” It means that the cited article does not mention or does not
contain this item.

4. EME for Environmental Remediation

Various methods, such as adsorption, photocatalysis, coagulation-precipitation, re-
verse osmosis, air flotation, ultrasonication, chemical oxidation, incineration, biochemistry
and EME, have been developed for the treatment of wastewater pollutants. As a new
technique, EME provides an innovative strategy for environmental remediation.

4.1. Removal of Inorganic Ions by EME

Golubenko and Yaroslavtsev [93] obtained a series of modified anion-exchange mem-
branes to form a pair of thin charged layers by utilizing the surface-sulfonated graft
anion-exchange membranes. The formation of the interfacial layer significantly improved
the selectivity of Cl− /SO24− and the resistance to humic acid adsorption. In electrodialysis,
the best surface-sulfonated anion-exchange membrane has a high Cl− /SO24− selectivity of
up to 6.4. It was established that the current density affects the Cl− /SO24− selectivity of
the surface-sulfonated anion-exchange membrane during the desalination process. The
obtained membranes exhibit antifouling characteristics towards high-molecular-weight
pollutants such as humic acids.
La Cerva et al. [94] proposed two coupled models for the Reverse Electrodialysis
(RED)-Reverse Osmosis (RO) and Electrodialysis (ED)-RO systems of seawater desalination.
In the electro-membrane pre-desalting process, the RED-RO consumed less energy than
the standalone seawater reverse osmosis (SWRO) for a wide range of external voltages.
The cost of ED-RO desalination was higher than that of SWRO. The RED-RO case offered
significant cost savings and had strong industrial application potential.
Gurreri et al. [95] combined an electric membrane process with RO technology to
desalinate real seawater in a pilot plant. The integrated plant recovered approximately
40% of its total water. In the ED-ED-RO, ED-RO, and shortcut reverse electrodialysis
(scRED)-assisted reverse electrodialysis (ARED)-RO setups, ED, scRED, and ARED were
investigated. When efficient ERDs are considered, the energy usage of SWRO was 20%
lower than the integrated plant’s minimal value. Coupling of electrolytic membrane
processes with RO processes may develop alternative, competitive industrial membranes
for seawater desalination.
Kuban [96] proposed a novel method for rapid and efficient desalination of tiny
volumes of brine samples using multiphase microelectroelectric membrane extraction (µ-
EME). The aqueous sample was the center solution sandwiched between two organic free
liquid membranes (FLMs) and two aqueous extraction solutions contained in a disposable,
clearly transparent extraction device containing microliter quantities of five immiscible
solutions. Target analytes were selectively prevented from migrating across the organic
phase by two FLMs, and analytes were kept in the sample. 1-pentanol was used as the
Membranes 2023, 13, 705 11 of 17

SLM, and extraction solutions were composed of 15 µL deionized water and 0.1 mol/L
NH4 OH. The driving force was 300 V and the extraction time was 60 min. From samples
with physiological NaCl values, more than 99.3% NaCl was removed. Each phase in the
extraction unit can have a unique volume, length, and composition. Simply changing
the volume of the FLM (decrease or increase) allows for the desalination of samples with
different salinities, resulting in faster and more stable desalination of low and high-salinity
samples, respectively. Sample desalination and targeted retention of specific analytes can
be achieved by fine-tuning the composition of the FLMs.
Nguyen and Pham [97] examined the operation of the reflux ion concentration po-
larization (ICP) desalination system. The ion transport mode, the control factors of ion
transport, and the ion transport in the desalination system were investigated in detail by
numerical simulation. An accurate numerical solution model of ion transport was estab-
lished. The process reduces the cost of the experiment. The actual reflux ICP desalination
technology is optimized and shows good promise in seawater desalination.

4.2. Removal of Organic Pollutants by EME

Olasupo et al. [16] prepared a classical polymer inclusion membrane (PIM) for the
removal of sulfamethoxazole antibiotics from aquatic samples by EME. The PIM was com-
posed of the base polymer cellulose triacetate, the carrier Aliquat® 336, and the plasticizer
dioctyl phthalate. Sulfamethoxazole was removed with a transport efficiency of 100% at
an extraction time of 15 h and a voltage of 50 V. Sulfamethoxazole was preconcentrated in
river water and wastewater samples with preconcentrate coefficients of 22.9–24.1.
Restan et al. [98] reported the EME of removing sodium dodecyl sulfate (SDS) from
samples that have been concentrated. The SLM was composed of 1.0% (w/w)Aliquat® 336
in 1-nonanol and the driving force was 5 V. SDS was removed from a 100 µL aqueous
sample using a 3 µL SLM, and the waste solution was 200 µL 0.01 mol/L NaOH in water.
In 30 min of operation, EME eliminated 100% of samples with 0.1% SDS. It was found that
SDS accumulated within the SLM during mass transfer and that replenishing the SLM or
increasing the surface area helped get around some of these problems.
Roman-Hidalgo et al. [18] successfully extracted seven p-hydroxybenzoates and three
fluoroquinolones simultaneously and selectively in a green electro-membrane extraction
process using chitosan biopolymer membranes as the carrier. In this process, 10 mL of
donor phase and 50 µL of acceptor phase were used, and the pH of both phases was
10. A voltage of 80 V was applied for 15 min extraction time. The enrichment factors
were estimated to be ≥90 for parabens and ≥50 for three fluoroquinolones. The limits
of detection were in the range of 0.2–1.1 µg/L. The method was successfully applied to
remove pharmaceutical contaminants from water samples (rivers, lakes, and lagoons). The
chitosan membrane used in the extraction process is a biodegradable and multifunctional
carrier that can be a good substitute for the commonly used polypropylene material.

4.3. Resource Recovery by EME

Yang et al. [99] proposed an electromembrane reactor for recycling and resource
recovery of flue gas desulfurization (FGD) residuals. First, by presenting the dimensionless
groups, a mathematical model was created to characterize the mass balance of the proposed
electromembrane reactor. Analysis of the model using dimensionless groups demonstrated
that current density, flow pattern, and initial acid and base concentration were crucial
factors in the optimization process, correlating with the outcomes of the experiments.
This technology, integrated with existing FGD facilities, will enable the transfer of costly
chemical processes to renewable resources and clean energy conversion processes.
Lin et al. [100] reported a Semi-dynamic EME for selective recovery of templates
in molecular imprinting. The molecularly imprinted samples prepared by precipitation
polymerization and native polymerization were used as the base template (propranolol)
with recoveries of 61% and 55%, respectively. By using UV-Vis, HPLC-UV, and MS measure-
ments, the selectivity of EME for template recovery from genuine samples was verified. This
Membranes 2023, 13, 705 12 of 17

confirmed the great potential of EME for the one-step selective extraction and purification
of ionizable compounds from complex samples.
Meng et al. [101] synthesized a novel PIM made of a compound carrier for bis(2-
ethylhexyl) phosphate (D2EHPA) and TBP, and the PIM enabled the first realization of the
EME of Li+ . It has been proven that as the applied electric field voltage rises, the mass
transfer rate of the system to Li+ increases dramatically. The driving force was 40 V, and
the thickness of the membrane was 200 µm. The mass transfer mechanism of TBP and
D2EHPA to Li+ was proposed.
Martoyan et al. [102] investigated a novel electro-membrane approach for 7 Li isotope
enrichment, which is a modified version of the amalgamation method for lithium isotope
enrichment. The cations of the 7 Li and 6 Li isotopes moved in solution at various rates in
response to an applied electric voltage between electrodes. The authors concluded that
most of the 6 Li isotopes were enriched in the mercury cathode, while the 7 Li isotopes
were concentrated on the top surface and in the working chamber. The mass spectrometer
inductively coupled plasma-mass spectrometry performed analyses to determine the iso-
tope ratio. The 7 Li isotope separation coefficient was 1.178, confirming the possibility of
enriching lithium isotopes using this method.
Trejo González et al. [103] selected a tubular renewable carbon-based material from
sugar cane harvest residues as an electroactive membrane contactor to recover fresh water
from brine. The finished carbon-based tubes had an outside dimension of 5.5 mm and
an internal diameter of 2.5; the lengths employed in this study ranged from 10 to 50 mm.
The driving force was 7 V, and the solute removal rate was higher than 99.4%. Membrane
contactors have lower thermal conductivity than most commercial membranes and show
promising applications in process thermal efficiency.

5. Conclusions
EME is an emerging green technology that is being developed for environmental
analysis and remediation. EME reduces organic solvent and sample volume, shortens
analysis time, and reduces operating costs. This review summarizes recent advances
in the selection of membrane materials, modification of membranes, types of organic
solvents, and applications in environmental pollutant detection and resource recovery.
To offer a full knowledge of the utilization of EME in environmental applications, the
impact of key process parameters has been highlighted. Operating factors including pH
of acceptor/donor phases, stirring rate, applied voltage, temperature, and SLM type are
supposed to enhance product recovery and selectivity. Under the appropriate conditions,
EME technology provides sensitive determination of environmental pollutants, effective
removal of pollutants from environmental wastewater, and rapid recovery of resources
from the environment.
However, there are still a few issues that need to be addressed. Numerous EME setups
have been created and taken into use for a variety of purposes over the last ten years. Most
of the equipment is homemade and not commercially available. With the development
of commercial and automated equipment, EME is sure to gain wider application in the
future. Another appealing approach in this field is the automation and minimization of
EME, even in complex matrices, based on novel and effective SLMs. In addition, more en-
vironmentally friendly and sustainable EME membranes are gaining increasing popularity
among researchers. The majority of currently published studies only use agarose-based
materials, primarily gel films, hence it’s critical to create novel, alternatives biodegradable
materials. EME is mostly used in environmental analysis to identify contaminants in soil
and water, while it is also starting to be applied to resource recovery and contaminant
removal. Nowadays, with the increasing diversity of contaminants in original samples, the
detection and removal of emerging contaminants (drugs, additives, dyes) also need to be
given special attention.
In summary, this review acknowledged the potential and capability of EME to be
used as a green extraction technique for the determination of organic pollutants and the
Membranes 2023, 13, 705 13 of 17

sustainable removal of toxic pollutants. According to this review, additional in-depth

studies that consider environmental factors more rationally than previous research works
are still required.

Author Contributions: Conceptualization, M.C.; resources, M.C. and F.X.; data curation, L.S., G.Z.,
X.W., M.F. and R.L.; writing—original draft preparation, L.S., M.C. and F.X.; writing—review and
editing, L.S., M.C. and F.X.; supervision, F.X.; project administration, M.C.; funding acquisition, M.C.
All authors have read and agreed to the published version of the manuscript.
Funding: This work was supported by the Innovation Project of Zhengzhou Tobacco Research
Institute (312020CR0300) and Scientific Research Program of Innovation Platform in State Tobacco
Monopoly Administration (312021AW0420).
Institutional Review Board Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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