Plasmonic Sensing with Molecular Imprinting Technology

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This entry is adapted from the peer-reviewed paper 10.3390/chemosensors11030203

Molecularly imprinted plasmonic nanosensors are robust devices capable of selective target interaction, and in some cases reaction catalysis. Recent advances in control of nanoscale structure have opened the door for development of a wide range of chemosensors for environmental monitoring. The soaring rate of environmental pollution through human activities and its negative impact on the ecosystem demands an urgent interest in developing rapid and efficient techniques that can easily be deployed for in-field assessment and environmental monitoring purposes. Organophosphate pesticides (OPPs) play a significant role for agricultural use; however, they also present environmental threats to human health due to their chemical toxicity. Plasmonic sensors are thus vital analytical detection tools that have been explored for many environmental applications and OPP detection due to their excellent properties such as high sensitivity, selectivity, and rapid recognition capability. Molecularly imprinted polymers (MIPs) have also significantly been recognized as a highly efficient, low-cost, and sensitive synthetic sensing technique that has been adopted for environmental monitoring of a wide array of environmental contaminants, specifically for very small molecule detection.

environmental monitoring plasmonics molecularly imprinted polymers

1. Introduction

Environmental contamination is a major crisis that has become an albatross for many global economies, such that the deliberate and unintended discharge of pollutants into the environment is a direct repercussion of the economic activities of humans ^[1]. The alarming rate of release of these toxic, chemical, and biological wastes thus poses a serious threat to human health and the ecosystem such that waterbodies, soil, air, aquatic species, and the food chain have all come under siege in recent times ^[2]. Due to the devastating impact of environmental pollutants on human health and the ecosystem, it is imperative and dire to develop rapid and sensitive analytical techniques to aid detection and assessment of the impact of these pollutants ^[3]. These rapid detection mechanisms could thus serve as and provide an early warning signal to support finding lasting solutions to mitigate and address this menace. Environmental monitoring employing rapid detection requires an effective approach to evaluating pollutants at extremely trace levels by employing highly efficient, sensitive, simple, and rapid analytical tools that can be used for real-life applications ^[1]^[3]. Although the gold standard approach and the most widely diverse analytical techniques used for environmental analysis include mass spectroscopy and chromatographic methods, their use for infield applications is hindered due to some drawbacks such as their expensive nature and complex instrumentation systems ^[4]. The advent of nanomaterials for environmental monitoring processes has broken several limitations of the conventional methods of detecting environmental contaminants as reported in numerous studies. Nanomaterial-based concepts that have been generally explored with promising potential for environmental monitoring include electrochemical sensors, surface plasmon resonance (SPR), and surface-enhanced Raman spectroscopy (SERS) sensing techniques ^[1]^[2]^[3]^[5].

The plasmonic features of noble metals enable them to adequately couple with electromagnetic radiation, thus creating a niche environment of electron plasma that potentially yields electromagnetic hot spots and is very useful for molecular sensing applications. In addition, the formation of these plasmonic hot spots serves as a catalyst for the detection of the vibrational characteristics of molecules at both nano and femtomolar concentrations ^[3]^[6].

SERS has been recognized as a promising and efficient analytical technique for the quantitative determination of a myriad of low molecular weight substances in complex matrices. This mechanism of SERS is solely based on the inelastic scattering of light, otherwise classified as Raman scattering. The SERS effect thus depicts the vibrational modes of the detected molecules, and its sensitivity is linked to the formation of an enhanced field of electromagnetic interactions between the analyte in proximity to the SERS substrates or the excited metal nanoparticles under resonance. It is thus noteworthy that the Raman signal enhancement is highly dependent on the chemical and electromagnetic enhancement potential of both the analyte and the substrate ^[7].

Localized surface plasmon resonance (LSPR) is an important plasmonic attribute of noble metals that results in the oscillations of surface charges that couple with electromagnetic waves. Thus, the wave propagation of these localized surface plasmons between the metal boundary and its adjacent dielectric is what results in this unique feature of the plasmonic effect ^[6]. However, an efficient LSPR effect significantly depends on the dielectric characteristics of the environment, the metal’s resonant wavelengths, as well as the geometry of the metal particles. Thus, tuning the shape and size of noble metal particles enhances their plasmonic, optical, and electrochemical characteristic properties for an array of sensing applications ^[6]^[8]. Hence, a plasmon wavelength shift is observed when there is a variation between the refractive index for a non-absorbent environment and the dielectric function of the surrounding ^[6]. It is thus evident that during sensing applications, the plasmon wavelength shift helps in signaling molecular binding events while the SERS probes and detects molecular components and their orientation on the surface of SERS nanomaterials ^[9].

Surface plasmons are generally oscillations of electrons that are propagated at the interface of plasmonic materials such as noble metals and a dielectric substance (for example, in an aqueous medium). The energy generated from surface plasmons is a function of the wavevector of light and the dielectric constants of both the dielectric and the plasmonic material ^[4]^[10]. The unique benefit of SPR and LSPR sensors is their label-free recognition mechanism and the variation in refractive indices that occur during the molecule detection on plasmonic surfaces. SPR and LSPR sensors are vital analytical tools, useful for environmental monitoring as they can detect molecular binding events between the target analytes and the plasmonic material and the difference between both SPR and the LSPR aligns with the scale of the length of the plasmonic material ^[4]^[10].

Nanoplasmonic sensors are excellent candidates for rapid analytical testing and environmental monitoring applications ^[5]^[11]. The SPR sensing effect on the surface of silver and gold, which are classical noble metals, is a result of the excited electrons in the conduction band that undergo coherent oscillations at the metal–dielectric interface by exposure to a wave of light. An important feature of the SPR effect is linked to sensitivity to changes in the refractive index surrounding the metallic structure, as well as the morphological characteristics of the nanostructure ^[6]^[12]. In addition, plasmonic sensors with the characteristic SPR effect have superior benefits due to their ease of preparation, cost-effectiveness as well as their unique label-free property which makes them excellent candidates for real-time monitoring applications. The suitability of SPR sensors for several fields of applications has been broadly centered on their non-invasiveness and their enhanced ability in localized sample probing. In addition, the synergistic coupling of plasmonic surfaces or SPR sensors with receptors such as molecularly imprinted polymers (MIPs) can enhance the sensitivity of these developed sensors for a broad range of sensing applications ^[7]^[13].

2. Surface Plasmon Resonance and Surface-Enhanced Raman Spectroscopy MIP Sensors

SPR and SERS are considered vital plasmonic features and are recognized as superior and ultrasensitive transduction and powerful readout technologies for a myriad of sensing applications ^[14]^[15]. These plasmonic features are more appealing to use by coupling with MIP chemosensors largely due to their capability of detecting various analytes such as pesticides, antibiotics, microorganisms, amino acids, and proteins at trace concentration levels ^[16]^[17].

Generally, an MIP chemosensor based on SPR has an integration of silver or gold nanocomposites coupled to it, which eventually relays a variation in refractive index and electron density at the MIP’s surface upon binding of the target analyte to the MIP ^[16]^[17].

Surface plasmon resonance (SPR): SPR could be defined as a collective oscillation of free electrons in the conduction band of a material that has an interfacial existence between two media with positive and negative dielectric permittivity constants that are triggered by incident light. The mobility of electrons thus generates an electromagnetic wave within and at the peripherals of the structure, therefore depicting a surface plasmon peak in the monitored region of the absorption spectrum ^[18]. For example, thin films coupled to metallic surfaces create an SPR signal upon analyte binding which is relayed to the SPR transducers, and the signal detected occurs due to a variation in the thickness and refractive index of the thin films. It is noteworthy that most noble metals such as silver and gold are a repository for surface plasmons; however, other suitable alternatives include chromium, copper, and titanium. In MIP sensors, their surfaces are usually functionalized by thiols via in situ thin film polymerization during the MIP’s pre-synthesis phase. A transducer integrated with an MIP sensor laced with silver or gold promotes the SPR signal during a binding event, whereby the applied incident light causes an incident angle shift due to the analyte binding effect altering the MIP layer’s refractive index ^[19].

Localized surface plasmon resonance (LSPR) also refers to the optical phenomenon whereby there is confinement of an electromagnetic wave or surface plasmon inside conductive nanoparticles such as in silver and gold; however, other suitable nanocomposites of platinum and palladium could also generate LSPR peaks. The LSPR effect occurs predominantly due to the free electrons in the metallic nanoparticles interacting with the incident light or electromagnetic wave, whereas the plasmonic frequency and intensity are dependent on multiple factors such as the dielectric constants of the medium and the morphological characteristic (size and shape) of the nanoparticles ^[18]^[19].

MIP–SPR sensors have found important use in many applications such as for the detection of proteins and biomolecules as well as detecting explosives. For example, histamine was successfully detected at a LOD of 25 µg/L by an SPR sensor that was spin-coated with MIP films ^[19]. Shrivastav et al. ^[20] developed a synergistic optical fiber MIP-SPR device for the determination of profenofos. This device had enhanced sensitivity and specificity for the target analyte with a LOD of 2.5 × 10⁻⁶ μg/L and the linear range for the detection was from 10⁻⁴ to 10⁻¹ μg/L. Another study by Saylan et al. ^[21] also developed an MIP-SPR sensor that was able to detect multiple pesticides such as atrazine, cyanazine, and simazine that were in aqueous form. The MIP sensor was highly selective and was thus able to detect the pesticide with LODs of 0.091, 0.095, and 0.031, respectively. Moreover, it was also observed that the sensor had the capability of being reused four times on average.

Surface-enhanced Raman Spectroscopy (SERS): SERS constitutes the enhancement of Raman scattering and is a very surface-sensitive process that occurs during a binding event and is stimulated by localized surface plasmon coupling with an electromagnetic wave or an incident polarized light on nanostructures or uneven metal surfaces. SERS relies on a signal detection mechanism and when incorporated into MIP-based sensors, this signal is amplified by plasmonic or chemical effects from Raman active molecules that depict a specific vibrational Raman spectrum ^[17]^[19]. SERS has distinguished its uniqueness from all other optical transduction mechanisms employed for MIP sensors due to its ability to ultra-sensitively and directly detect targets at solid and liquid interfaces ^[22]^[23].

Interestingly, SERS measurements can be depicted in coordination with Raman active molecules as well as employed with the LSPR mechanism. Although the SERS mechanism is not completely understood, there are two schools of thought as evidenced in the literature. The first concept is linked to the formation of a chemical bond due to a charge-transfer complex between the metallic structure and the target analyte, thus enhancing its polarization effect. The second concept, on the other hand, revolves around the theory of electromagnetism, in conjunction with the LSPR effect around the surface of the nanoparticles ^[19]. A summary of some efficient MIP sensors developed with SPR and SERS for the detection of various environmental contaminants is outlined.

Furthermore, SERS have been efficiently employed for the non-destructive and rapid identification of a wide array of matrices inclusive of chemical and biological analytes. For example, MIP sensors have successfully explored the efficiency of SERS in detecting histamine (HIS) in canned fish and its reliability and accuracy were unmatched with HIS results ranging from 3 to 90 ppm ^[24]. The technique of SERS involves an inelastic scattering phenomenon and thus can be used to depict the structural properties of a molecule ^[25]. Classical noble metals such as silver and gold nanocomposites provide a synergistic SERS effect as these are vital substrates that influence the displayed Raman spectra ^[25]. The effectiveness of SERS could also be significantly enhanced by coupling it with other techniques such as labeling techniques, colorimetry, and microfluidic systems ^[25]. In addition, for enhanced accurate analytical sample characterization, SERS could be synergistically used with procedures such as infrared spectroscopy, X-ray photoelectron spectroscopy (XPS), nuclear magnetic resonance (NMR), and mass spectrometry ^[18]. For example, an MIP–SERS Solid-Phase Extraction (SPE) with silver nanoparticles as a SERS substrate was able to efficiently and rapidly detect 2,4-dichlorophenoxyacetic acid in milk samples ^[26].

Similarly, another study by Feng et al. ^[27] employed an MIP chemosensor developed on the principle of SERS for the selective detection of thiabendazole in orange juice samples with LOD 4 ppm. The MIP–SERS sensor setup constituted a SPE cartridge that was laced with the MIPs as sorbents. Interestingly, this sensor system was highly sensitive and very rapid with the complete analytical detection process occurring within twenty-three (23) minutes.

3. Nanomaterial-Based Sensors for Environmental Monitoring

Nanomaterials have become attractive elements for the development of sensors for environmental applications due to their unique surface chemistry and functional properties including their potential to detect environmental pollutants at low concentrations ^[28]. These nanomaterials are endowed with tunable physico-chemical properties and desirable characteristics such as enhanced catalytic potential, high surface-to-volume ratio, as well as enhanced surface reactivity. These intrinsic properties of nanomaterials promote their suitability as efficient nanosensors for environmental monitoring applications ^[29]. Nanomaterials could thus play two significant roles in sensors, which include a strong affinity for absorption and sensitive signal transduction. For example, graphene or carbon nanotubes (CNTs) possess a strong adsorptive capacity that could enhance the detection of the targeted analyte; in addition, metal nanoparticles such as gold (Au) or silver (Ag) could efficiently amplify the signal transduction linked with the detection of the targeted analyte.

Another salient application of nanocomposite materials involves Au and Ag nanoparticles for the design of colorimetric and optical sensors, as they function on the principle of color change and excitation of LSPR when a chemical analyte is detected ^[29]. Nanosensors generally possess superior performance compared to conventional sensors due to their high level of sensitivity, specificity, and rapid response time ^[30]^[31]^[32]. Consequently, nanocomposite materials can be functionalized as nanosensors for ultrasensitive or trace element detection of environmental pollutants in complex matrices ^[28]. The properties of nanomaterials coupled with analytical signal detection techniques such as SERS, fluorescence, and electrochemistry have caused the field of nanosensors to evolve significantly over the years ^[28]^[29].

To date, CNTs, quantum dots, graphene, silicon nanowires, Au, and Ag nanoparticles have been significantly exploited in several studies for the detection of environmental contaminants including pesticides. Graphene and CNTs have been efficiently employed as field-effect transistor (FET) sensors for the detection of heavy metals and pesticides due to their suitable and excellent electrically conductive property ^[33]. Silver and gold nanoparticles have historically exhibited enhanced extinction coefficients and are suitable candidates as bio- and chemosensors for a wide array of environmental monitoring applications. Generally, the effect of plasmonic coupling in metallic nanoparticles induces electromagnetic enhancement, thus promoting SERS signals of the analytes to be captured and detected in the nanosensors and very much useful for single-molecule sensitivity ^[34]. Several studies have highlighted the detection of pesticides with nanomaterial-based sensors. For example, Moraes et al. ^[35] successfully detected carbaryl (1.09 ± 0.02 μg/L) in natural water samples by using a multi-walled carbon nanotube/cobalt phthalocyanine modified electrode. Methyl parathion was also detected in fruits and vegetables with the synergistic coupling of silver and graphene nanoribbon nanocomposite-modified screen-printed electrode ^[36]. Another study by Liao et al. ^[37] yielded a sensitive fluorescence immunoassay sensor device that was composed of CdSe/ZnS Quantum dots. The sensor efficiently detected triazophos in apple, pear, cucumber, and rice samples. Au nanoparticles were also used as signal enhancers in optical biosensors and efficiently determined a cocktail of OP compounds (edifenphos, iprobenfos, and diazinon) by a change in coloration of the aggregated Au nanoparticles when they were in contact with the targeted OP compounds. Outstanding results due to the Au nanoparticles were recorded as 27.9 ppb, 53.6 ppb, and 53.3 ppb LODs for edifenphos, iprobenfos, and diazinon, respectively ^[38].

4. Nanoparticle MIPs (NanoMIPs) for Chemosensing of Environmental Pollutants

The quest to enhance analytical sensing techniques has yielded tremendous results with the adoption of MIP systems, especially in the chemosensor and bioassay sectors. The robustness of MIPs with the integration of nanoparticles broadens the functionality of the chemosensor for a wide range of applications. Consequently, the MIP chemosensor should possess the below-recommended features ^[17]:

(i): High specificity and enhanced affinity that has unparalleled recognition characteristics when coupled with a transducer.
(ii): An intensely sensitive transducer for monitoring and processing the binding potential between the monomer and the imprinted cavities.

MIPs have also distinguished their usefulness in chemical sensing such that targeted analytes in the MIP chemosensors generate physicochemical changes during binding reactions which trigger signals that are transduced and confirmed for the quantitative or qualitative attribute of the toxicant determined. Typical aspects of these transduction signals include a change in optical or fluorescence intensity, and the most employed signal transduction includes SERS, SPR property conductometry, voltammetry, potentiometry, and amperometry ^[17]. NanoMIPs have a promising potential to detect a myriad of environmental pollutants such as antibiotics in various matrices.

Interestingly, MIPs can be synthesized in different modes such as in the form of nano- or microparticles or as films and membranes. In context, nanoparticle MIPs present significant superiority compared to the other forms of bulk material MIPS due to their enhanced binding kinetics, loading capacity and chemical reactivity potential ^[39]^[40]. This phenomenon could be attributed to the concept of ‘small is big’, which implies nanoparticles possess a larger surface-to-volume-ratio per unit weight of the polymer matrix ^[17]. Consequently, the functionality of the MIP system is enhanced by the nanoparticles such that the affinity of the imprinted cavities for the analytes of interest, the kinetics of binding, template removal, as well as molecular recognition characteristics are highly stimulated. Scientific researchers and several authors have determined that nanoparticles embedment in MIPs is very promising, and as such it is considered in sensing assays or for sensor, therapeutic and diagnostic applications. For example, D’Aurelio and coworkers ^[41] developed a highly sensitive nanoMIP-SPR-based sensor for the detection of β-lactoglobulin. Ashley et al. ^[42] also synthesized a nanoMIP sensor for the detection of α casein based on the property of SPR. NanoMIPs have also been efficiently developed as biomarkers for the detection of fucose and mannose ^[43].

For the environmental monitoring of OPPs, novel dual-templated nanoMIPs developed by Abbasi Ghaeni and coworkers were very efficient in detecting diazinon, malathion, glyphosate and dichlorvos in water treatment samples. The nanoMIPs were prepared by the precipitate polymerization technique and the template molecules were the same as the evaluated OPPs. An enhanced binding affinity of the MIP nanoparticles for the detected OPPs were observed in comparison to the non-imprinted polymer nanoparticles ^[44].

Another fascinating outlook of MIPs is their synergistic interaction with nanoparticles for the development of detection assays. Interestingly, these nanoMIP detection assays have optical and colorimetric properties, thus they are suitable and promising candidates for a wide range of applications ^[16]. For example, Piletska et al. ^[45] developed a novel magnetic nanoMIP assay for pepsin detection. In their study, pepsin was the template or target molecule which was synthesized based on a solid-phase technique. The readout of the nanoMIP assay and its sensitivity was also linked to the inclusion of fluorescent polystyrene beads which yielded excellent results and detected pepsin in the quantifiable range between 5 and 50 μg/mL.

In addition, nanoMIPs have become efficient vital tools for the rapid detection of environmental pollutants such as the OPPs, diazinon in food and drinking water. This was evidenced by the development of an MIP nanoparticle-based electrochemical sensor for the analytical determination of diazinon in apple fruits and well water samples ^[46]. The precipitate polymerization technique was employed in synthesizing both the MIP and the non-imprinted polymer (NIP). In addition, the MIP nanoparticles were immobilized on a carbon paste electrode and the square wave voltammetry was used for the analytical determination of diazinon in the evaluated samples. It was reported that the sensor was highly efficient for detecting this OPP in the tested samples and the reported LOD of 5.43 × 10⁻⁹ M was obtained. Furthermore, the recovery rate of the developed sensor was very promising and was in range of 99.06 to 99.16% ^[46].

Another study by Wu et al. ^[47] demonstrated the colorimetric quantitative detection of cartap (pesticide) residue in tea beverages by employing a silver nanoparticle sensor coupled with a magnetic MIP microsphere system. In their design, cartap was the centralized template molecule, mesoporous SiO₂ was the intermediate shell, and the recognition element was Fe₃O₄@mSiO₂@MIPs, functional monomer (methacrylic acid), and Fe₃O₄ was used as the core-shell. The developed nanoMIP thus selectively eluted cartap from the spiked tea samples and the incorporated silver nanoparticles confirmed the quantitative presence of the pesticide (0.1–5 mg/L with LOD 0.01 mg/L) as measured by UV–vis spectroscopy.

In addition, a study by Mankar et al. ^[48] also developed an efficient nanoMIP system that selectively adsorbed and detected arsenic in groundwater. In their design, polymethacrylate was used as the functional monomer, and imprinting was achieved by the complex of arsenic and fluorescein. The resultant nanoMIP demonstrated a high arsenic adsorption capacity (49 ± 7 mg/L) and had a recovery rate of 98% when the nanoMIP was thoroughly washed with 0.1 M HNO₃ solution.

Over the recent years, a research laboratory has developed and demonstrated that organic compounds acting as chemosensors distinctively detected different OPPs through fluorescence emissions. In such work, Guo et al. ^[49] confirmed that three different OPPs, namely fenthion, malathion, and ethion, uniquely provided fluorescence emissions by binding to two phenanthroline derivatives which include (i) benzodipyrido [3,2-a:2*,3*-c] phenazine (BDPPZ) and (ii) 3,6-dimethylbenzodipyrido-[3,2-a:2*,3*-c] phenazine (DM-BDPPZ), respectively. It was thus confirmed that the BDPPZ and the DM-BDPPZ selectively bounded to the evaluated OPPs and had a significant limit of detection (LOD) of 10⁻⁸ M, 10⁻⁹ M, and 10⁻¹² M, respectively, for fenthion, malathion, and ethion. The promising outcome of these results confirmed the potential for these chemosensors to selectively detect OPPs and be employed for environmental monitoring purposes.

Obare et al. ^[50] evaluated the effectiveness of dimethyl-[4-(2-quinolin-2-yl-vinyl)-phenyl]-amine (DQA), an azastilbene derivative, as an efficient chemosensor using fluorescence spectroscopy for the detection of four distinct OPPs, namely ethion, malathion, parathion, and fenthion, respectively. It was observed that fluorescence quenching was evident in all cases at a wavelength of 530 nm for ethion, malathion, and parathion, except no quenching was observed for the fenthion OPP when they were titrated with DQA.

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Subjects: Nanoscience & Nanotechnology; Chemistry, Analytical

Contributors MDPI registered users' name will be linked to their SciProfiles pages. To register with us, please refer to https://encyclopedia.pub/register :

Raphael D. Ayivi

Bukola O. Adesanmi

Eric S. McLamore

Jianjun Wei

Sherine O. Obare

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Update Date: 31 Mar 2023

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