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Lasarte-Aragones, G.; Lucena, R. Effervescence-Assisted Microextraction. Encyclopedia. Available online: https://encyclopedia.pub/entry/6372 (accessed on 20 June 2024).
Lasarte-Aragones G, Lucena R. Effervescence-Assisted Microextraction. Encyclopedia. Available at: https://encyclopedia.pub/entry/6372. Accessed June 20, 2024.
Lasarte-Aragones, Guillermo, Rafael Lucena. "Effervescence-Assisted Microextraction" Encyclopedia, https://encyclopedia.pub/entry/6372 (accessed June 20, 2024).
Lasarte-Aragones, G., & Lucena, R. (2021, January 13). Effervescence-Assisted Microextraction. In Encyclopedia. https://encyclopedia.pub/entry/6372
Lasarte-Aragones, Guillermo and Rafael Lucena. "Effervescence-Assisted Microextraction." Encyclopedia. Web. 13 January, 2021.
Effervescence-Assisted Microextraction
Edit

Effervescence-assisted microextraction emerged in 2011 as a new alternative in this context. The technique uses in situ-generated carbon dioxide as the disperser, and it has been successfully applied in the solid-phase and liquid-phase microextraction fields. This minireview explains the main fundamentals of the technique, its potential and the main developments reported.

dispersion micro-solid phase extraction

1. Introduction

The contact surface area between the donor (sample) and the acceptor (extractant) is a critical variable in the context of microextraction techniques [1]. The efficient dispersion of the extractant phase into the sample in the form of a fine suspension of micro/nano particles or drops is the most common approach to enhance the close contact between phases [2]. Several strategies, both in the solid-phase and liquid-phase microextraction contexts, have been proposed. These strategies can be generally divided into two main groups depending on the use of a external energy source [3][4] or chemicals [5][6] to achieve this dispersion.

In 2011, a new dispersion strategy was proposed by Lasarte-Aragonés et al. [7] and, since then, it has been developed and applied by many different groups worldwide. The technique is based on the in situ generation of carbon dioxide because of the reaction between a carbon dioxide donor and a proton donor in the so-called effervescent reaction. The CO2 bubbles generated produces an efficient dispersion of the extractant phase into the sample. The technique has been successfully applied to the solid-phase and liquid-phase microextraction contexts, as a green, cheap, and simple alternative.

2. Effervescence-Assisted Dispersive Micro-Solid Phase Extraction

Dispersive solid phase extraction (DSPE) is based on the dispersion of a solid sorbent into the sample of interest proposed by Anastassiades [8] as clean-up method aimed to remove interferences from the matrix, aided by vortex agitation. This kind of cleanup strategy later received the name of QuEChERS, an acronym for its advantages: quick, easy, cheap, effective, rugged, and safe and is now commercially available as a sample treatment strategy [9].

The miniaturized version is usually named dispersive micro-solid phase extraction (DµSPE). The cornerstone of DµSPE is the dispersion of the sorbent (extractant phase) in the sample. The process must take into consideration the nature and properties of the sorbent (polarity, micro or nano-size, aggregation) and can be achieved by physical or chemical means. Physical dispersion is typically assisted by an external energy source such as ultrasound irradiation [10] or vortex agitation [11]. Chemical dispersion is aimed to improve dispersibility by using a water-miscible organic solvent such as acetonitrile or methanol [12].

The first effervescent-based approach for this alternative is based on the fabrication of a tablet containing a commercial sorbent (OASIS-HLB) and reaction precursors (sodium carbonate as CO2 source and sodium dihydrogen phosphate as proton donor) [7]. The tablet containing all the elements was then introduced into the aqueous sample, and the sorbent is effectively dispersed by the in situ-generated gas bubbles. The alternative is designed to provide all the elements to perform the extraction process on-site, avoiding the use of a disperser solvent (minimizing environmental impact and waste generation) or external apparatus (such as vortex or ultrasounds). In fact, the first implementation of the technique employs a syringe as both sample-collection and extraction vessel device. The effervescent sorbent tablet is placed inside the syringe and the extraction process starts once the sample is aspirated. The dispersed sorbent can be easily recovered by a syringe filter and eluted before analysis. The method was employed for the determination of nitroaromatic compounds in water samples. Its analytical performance was comparable to other SPE alternatives for the same analytical problem, but in a simpler and rapid fashion. Analyte partition equilibrium is not affected by the effervescence process, and different sorbents can be used according to the target analytes.

The potential of effervescent tablets was later demonstrated in the effective dispersion of a nanometric sorbent, multiwalled carbon nanotubes (MWCNTs), in aqueous matrices [13], which are known for their limited dispersibility due to their trend to aggregation. The use of effervescent tablet (102 mm ID) was responsible for the efficient dispersion of the unmodified sorbent, resulting in more effective than mechanical agitation. By this means, a small amount of sorbent (7.5 mg) can be successfully dispersed in a large sample volume (100 mL) without the assistance of any external apparatus or energy source. The proposed alternative combined with Liquid Chromatography-Diode Array Detector (LC-DAD)

3. Effervescence-Assisted Dispersive Liquid-Phase Microextraction

Dispersive liquid–liquid extraction (DLLME), proposed by Rezaee et al. in 2006, is based on the efficient dispersion of an extractant solvent into the sample [14]. In the typical approach, this dispersion is aided by a disperser solvent that is miscible with both the sample and the extractant phase, which is recovered by centrifugation. The use of an organic solvent as the disperser has two main shortcomings. On the one hand, the volume of disperser solvent is in the mL range, and, therefore, DLLME cannot be completely considered a microextraction technique. On the other hand, the disperser solvent is mixed with the aqueous sample, increasing the analytes’ solubility in the donor phase, reducing its transfer to the extractant phase. The need for a disperser solvent can be reduced if an external energy source, like US [36] and vortex [5], is used.

Lasarte-Aragones et al. proposed the adaptation of effervescence extraction to the LPME context in 2014 [15]. Effervescence-assisted DLLME (EA-DLLME) consists of the in situ production of carbon dioxide due to the reaction of sodium carbonate (previously added to the sample) and the disperser solvent (acetic acid), which also contains the extractant phased. The reaction also generates sodium acetate that contributes to the ionic strength and may produce a salting-out effect. In this preliminary work, magnetic nanoparticles were added to the acetic acid-extractant mixture and used to recover the extractant from the sample avoiding the centrifugation process. The extractant solvent, 1-octanol, is recovered by the interaction of the alcohol group with residual hydroxyl groups on the surface of the nanoparticles.

4. Developments of Effervescence-assisted microextraction

Since its introduction, many researchers have expanded the applications of the concept to a variety of sorbents and solvents in different matrices, demonstrating the wide range of applicability of the technique. A detailed and complete review of these methodologies can be found in the recent publication by our research group [16]. The main contributions to the technique are presented in Table 1.

Table 1. Applications based on the use of effervescence-assisted microextraction.

Effervescent agents

Extractant

Sample

Analytes

Notes

Ref

CO2 donor

H donor

Type

Amount

Na2CO3

NaH2PO4

Oasis HLB

Water

10 mL

Nitroaromatic compounds

The tablet is placed on the syringe used as extraction vessel. Effervescence occurs upon sample aspiration inside the vessel. Sorbent with extracted analytes is recovered by syringe filter.

[7]

Na2CO3

NaH2PO4

MWCNTs

Water

100 mL

Triazines

Nanotubes are only effectively dispersed in tablet format with no additional organic solvent.

[13]

Na2CO3

NaH2PO4

G-MWCNTs-COOH

Hawthorn herb

200 mL

Natural antioxidants

The tertiary tablet is prepared by blending the ingredients and applying pressure. Different types of nanotubes were evaluated.

[17]

Na2CO3

NaH2PO4

Mesoporous hybrid materials (PCMA-60)

Root extracts

20 mL

Tanshinones

The tertiary tablet is prepared by blending the ingredients and applying pressure. Higher amounts of sorbent (13 mg) produce aggregation and decrease in extraction efficiency

[18]

Na2CO3

NaH2PO4

β-cyclodextrin/attapulgite composite

Water

7 mL

Pyrethroids

The tablet is placed on the syringe used as extraction vessel. Effervescence occurs upon sample aspiration inside the vessel. Sorbent with extracted analytes is recovered by syringe filter

 

[19]

Na2CO3

NaH2PO4

Magnetic attapulgite/polypyrrole nanocomposites

Honey

100 mL (diluted)

Pyrethroids

The tertiary tablet is prepared by blending the ingredients and applying pressure. Magnetic properties of the sorbent are used to facilitate sorbent recovery.

[20]

Na2CO3

NaH2PO4

IL-Magnetic-β-cyclodextrin/attapulgite composite

Honey and Juice

8 mL

Fungicides

The tertiary tablet is prepared by blending the ingredients and applying pressure. The sorbent is easily recovered using an external magnet.

[21]

Na2CO3

NaH2PO4

NiFe2O4 MNPs

Seafood extracts

30 mL

Heavy metals

The tertiary tablet is prepared by blending the ingredients and applying pressure. The sorbent is easily recovered using an external magnet.

[22]

Na2CO3

Citric acid

Fe3O4/chitosan-Se MNPs

Sausage extracts and Water

10 mL

Heavy metals

The tertiary tablet is prepared by blending the ingredients and applying pressure. The sorbent is easily recovered using an external magnet. Selenium increase extraction potential for metal ions

[23]

Na2CO3

Citric acid

Dopamine-modified magnetic graphene oxide

Sausage extracts and Water

100 mL

Metal ions

The tertiary tablet is prepared by blending the ingredients and applying pressure. The sorbent is easily recovered using an external magnet. Dopamine enhances extraction capacity.

[24]

Na2CO3

Citric acid

Dopamine-carbon graphite nitride nanosheets

Oil and water samples

100 mL

Metal ions

The tertiary tablet is prepared by blending the ingredients and applying pressure. Sorbent with extracted ions is separated by centrifugation.

[25]

Na2CO3

Citric acid

Fe3O4@SiO2@N3 MNPs

Urine and pharmaceutical wastewater

10 mL

Antidepressant drugs

The tertiary tablet is prepared by blending the ingredients and applying pressure. The sorbent is easily recovered using an external magnet. Nitrogen-rich surface increases adsorption capacity.

[26]

Na2CO3

Tartaric acid

Ni-based N-doped Graphene tubes

Deproteinized milk

5 mL

Bisphenols

The tertiary tablet is prepared by blending the ingredients and applying pressure. Magnetic properties of Ni-based tubes are used to facilitate sorbent recovery.

[27]

Na2CO3

NaH2PO4

Core-shell magnetic COF

Water, beverages and biosamples

5 mL

Endocrine

disruptors

The tertiary tablet is prepared by blending the ingredients and applying pressure. Magnetic properties of the sorbent are used to facilitate sorbent recovery.

[28]

NaHCO3

NaH2PO4

benzo-15-crown-5

C. fraxini medicinal plant

-

Coumarins

The procedure consists of matrix solid-phase dispersion extraction.

[29]

NaHCO3

NaH2PO4

CNT /polystyrene-divinylbenzene composite

Biosamples

1 mL (for liquid samples) and 6 mL (for reconstituted solid samples)

Alkaloids and flavonoids

The extractant is prepared as effervescent powder (sodium bicarbonate) inside a pipette tip. The proton donor is added to the aqueous sample before manual withdrawal. The effervescence occurs inside the pipette tip dispersing the sorbent.

[30]

NaHCO3

NaH2PO4

IL-coated core-shell SiO2@Fe3O4 MNPs

Plasma

10 mL (diluted)

Betablockers

Synthesized sorbent (IL-SiO2@Fe3O4) added separated to effervescent precursors shows better extraction efficiency than adding the components mixed (non-immobilized IL).

[31]

NaHCO3

NaH2PO4

[3C6C14P] [BF4]

Water

10 mL

Benzoylurea insecticides

A tertiary tablet containing the effervescence precursors and the IL is prepared.

After the extraction, the solvent is recovered as a solid in the upper part of the centrifugation tube.

[32]

Na2CO3

NaH2PO4

Ionic liquid nanofluid

Honey and tea

8 mL (honey is 1:10 w/v diluted)

Acaricide

A tertiary tablet containing the effervescence precursors and the IL nanofluid is prepared.

The solvent is recovered by centrifugation.

[33]

Na2CO3

NaH2PO4

[HMIM] [PF₆]

Food samples

10 mL (pretreated sample)

Selenium

The ionic liquid is added to the tablet that also contains the effervescence precursors and magnetic nanoparticles.

[34]

Na2CO3

NaH2PO4

[HMIM] [NTf2]

Water

8 mL

Fungicides

The ionic liquid is added to the tablet that also contains the effervescence precursors and magnetic nanoparticles.

[35]

Na2CO3

NaH2PO4

[BMIM] [PF₆]

Water and milk

7 mL (pretreated sample)

Polybrominated diphenyl ethers

The ionic liquid is added to the tablet that also contains the effervescence precursors and magnetic nanoparticlesFe3S4 are used instead of common Fe3O4.

[36]

Na2CO3

Tartaric acid

[HMIM] [BF4]

Urine and serum

7 mL (diluted and pretreated sample)

Endogenous steroids

The ionic liquid is added to the tablet that also contains the effervescence precursors and magnetic nanoparticles

After the extraction NH4PF6, is added to make the IL recovery easier.

[37]

Na2CO3

NaH2PO4

[BMIM]2 [Br]2

Meat

5 mL (pretreated sample)

Polycyclic Aromatic Hydrocarbons

The tablet contains the effervescence precursors, the IL, the metathesis reagent, and the magnetic nanoparticles

NiFe2O4 nanoparticles are used.

[38]

Na2CO3

HCl

[HMIM] [PF₆]

Milk

8 mL (pretreated sample)

Pyrethroids

The ionic liquid is added to the tablet that also contains the CO2 source and magnetic nanoparticles. HCl is added previously to the sample.

The magnetic nanoparticles simplify the IL recovery as it coats the surface of the nanomaterial.

[39]

NaHCO3

[BMiM][HSO4]

Tea beverage

5 mL

Triazine herbicides

The IL acts as solvent and H+ donor.

After the extraction, NH4PF6 is added to make the IL recovery easier. The IL is recovered by centrifugation.

[40]

Na2CO3

NaH2PO4

[BMIM][FeCl4],

Vegetables

10 mL (pretreated sample)

Arsenite and arsenate

The tablet contains the effervescence precursor and the magnetic IL.

[41]

NaHCO3

Oxalic acid

Sodium nonate

Water

1 L

Steroids

The tablet contains the effervescence precursor and the solvent.

Two tablets are added to the sample

[42]

Na2CO3

Sulfuric acid

Fatty acid

Several samples

10 mL (pretreated sample)

Antibiotics

The effervescence precursors are added as solutions

The fatty acid is recovered by the solidification of floating drop technique.

[43]

Na2CO3

Sulfuric acid

Fatty acid

Food samples

6 mL (pretreated sample)

Azo dyes

The effervescence precursors are added as solutions.

[44]

NaHCO3

Citric acid

Sodium octanoate

Beverage

5 mL

Endocrine disrupting chemicals

The tablet contains the effervescence precursor and the solvent.

The fatty acid is recovered by the solidification of floating drop technique.

[45]

NaHCO3

Citric acid

Sodium hexanoate

Water

5 mL

Triazine herbicides

Magnetic nanoparticles are added to the tablet to aid the recovery of the sample after the extraction.

[46]

NaHCO3

Acetic acid

DES containing Aliquot 336 and decanoic acid

Food

8 mL (pretreated sample)

Synthetic dyes

DES is dissolved in acetic acid and injected into the sample containing NaHCO3.

[47]

Na2CO3

NaH2PO4

DES containing choline chloride and phenol

Water

25 mL

Copper

An effervescent tablet is place in the extraction vessel. Later, the sample and the DES are introduced into the vessel.

[48]

NaHCO3

Citric acid

DES containing hexyltrimethylammonium bromide and 1-dodecanol

Water

5 mL

EDC

Fe3O4 coated with activated carbon nanoparticles is added to recover the solvent after the extraction.

[49]

NaHCO3

Citric acid

DES containing thymol with octanoic acid

Liquid samples

5 mL

Fungicides

The DES is recovered by solidification of DES.

[50]

Na2CO3

Formic acid

DES containing formic acid and menthol

Liver

10 mM (pretreated sample)

Ketoprofen, diclofenac

The HBD acts as proton donor in the effervescent reaction while the HBA acts as the solvent.

[51]

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