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Environmental Chemistry Letters (2018) 16:161–182 https://doi.org/10.1007/s10311-017-0674-7

R E V I E W

Nanosensors and nanobiosensors in food and agriculture

Anup K. Srivastava1 · Atul Dev1 · Surajit Karmakar1

Received: 16 October 2017 / Accepted: 23 October 2017 / Published online: 21 December 2017 © Springer International Publishing AG 2017

Abstract The food and agriculture sector controls the economic growth of a developing country. The food industries have practices of growing crops, raising livestock and sea foods, food processing and packaging, regulating production and distribution with quality and safety. The process control and monitoring quality are crucial steps. Here we review nanosensors and nanobio- sensors as alternative of classical quantification methods. Nanoscale dimensions of metal nanoparticles, metal nanoclusters, metal oxide nanoparticles, metal and carbon quantum dots, graphene, carbon nanotubes, and nanocomposites expand the sensitivity by signal amplification and integrate several novel transduction principles such as enhanced electrochemical, optical, Raman, enhanced catalytic activity, and superparamagnetic properties into the nanosensors. The electrochemical nanosensors, optical nanosensors, electronic nose and electronic tongue, nanobarcode technology, and wireless nanosensors have revolutionized the sensing in food and agriculture sectors with multiplex and real-time sensing capabilities. Despite previous success stories of the remunerative health sector, the approaches are transferred subsequently to food and agri- culture sector; with potential application in detection of food contaminants such as preservatives, antibiotics, heavy metal ions, toxins, microbial load, and pathogens along with the rapid monitoring of temperature, traceability, humidity, gas, and aroma of the food stuff.

Keywords Nanosensors and nanobiosensors · Agriculture · Food quality · Precision agriculture · Electrochemical nanobiosensors

Introduction

Food and agriculture sectors are two promising area decid- ing the sustainability and economic growth of a country. The food engineering involves the use of pH, temperature, and solvent activity that advances the choice of raw materials, formulations of food products, provides a thrust to manufac- turing and bio processing, and enhances the shelf-life of the food (Heldman and Lund 2011). The principle of sustainable agriculture to meet our present need without compromising the resources for future generation depends on two pros- pects; first, the agriculture practices should be self-sustained by conservation of protective resources, i.e., maintaining soil fertility, protecting groundwater, developing renewable energy and the alternative for tolerating the consequences of climate change. Second is considering the sustainability

by managing the nearby urban area with proper recycling of sewage waste, developing rural employment and con- tributing to construct a rural landscape (Lichtfouse et al. 2009). The affirmative agriculture productivity is compro- mised with the consequences of soil erosion, groundwater pollution, river eutrophication, development of weed, and resistant to the chemical control, thus affecting the environ- ment (Lichtfouse et al. 2005). The implementation of the nanotechnology is promising and provided a new edge to the agrotechnology, improved irrigation and fertilizer uti- lization, and enhanced the food production and processing, packaging and storage. The nanotechnology-based sensing gained enormous momentum and provided broad-spectrum application in food and agriculture sector (Neethirajan and Jayas 2011).

Nanotechnology puts the impetus to revolutionize the area of diagnostics in health, medicine, food, environment, and agriculture sector, transitioning theoretical aspects into the practical output. In turn, it plays a crucial role in the development and innovation which enhances the sensitivity and attributes the nanosensors and nanobiosensors-based

* Surajit Karmakar [email protected]

1 Institute of Nano Science and Technology, Habitat Centre, Phase-10, Sector-64, Mohali, Punjab 160062, India

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applications (Momin et al. 2013). The generalized definition of a chemical sensor is a device that transforms chemical information, ranging from the concentration of a particu- lar sample component to total composition analysis, into an analytically useful signal. However, biosensors are defined as an analytical device for the quantitative detection of an analyte with a biologically active element such as an anti- body, enzyme, oligonucleotide, or receptor attached to the surface of a transducer. The biological recognition molecule interacts with target compound, and the physical transducer converts the biological response to a detectable signal, quantitates as redox changes, and detects electrochemi- cally, optically, acoustically, mechanically, calorimetrically, or electronically, which can be correlated with the analyte concentration (Sharma and Rogers 1994). The characteristic of a biological entity to interact with a particular analyte or substrate is employed in the designing of biosensors. Spe- cifically, the nanobiosensors constitute transducer based on nanomaterials, having physical nanoscale confinement or nanofabrication of nanoparticles or nanostructured surfaces. Biosensors cover well-established bioanalytical techniques, while nanobiosensors with integration of nanotechnology revolutionize this field with potential alternatives by mini- mizing the load of standard laboratory methods and proto- cols, along with the benefit of quick response time, enhanced sensitivity, robustness, and portability for a point on use (Gomes et al. 2015).

The present review emphasizes various nanotech- nological approaches in construction and designing of new nanosensors and nanobiosensors. The nanocon- fined metallic nanoparticles like gold nanoparticle, silver

nanoparticle; magnetic nanoparticle, quantum dots, upcon- version nanoparticle, graphene oxide, single- and multi- walled carbon nanotubes, nanostructure-based sensors in the e-nose and e-tongue, and wireless nanosensors func- tionalization or fabrication have been used to achieve the enhanced sensing. Based on transducer, the nanosensors, bionanosensors, electrochemical nanosensors, optical nanosensors, wireless nanosensors, nanobarcode technol- ogy are discussed in detail. Nanosensors and nanobio- sensors have potential application in the food sector as in monitoring food processing, food quality assessment, food packaging, food storage, monitoring of shelf-life and viability, indicator of food safety and microbial contamina- tion, toxin and residual contamination in food. The major implication in the area of agriculture is physical moni- toring of temperature, humidity, soil quality and fertility, sensing microbiological microenvironment of the soil, indicator for seed viability and shelf-life, response sensors for irrigation and safety in agronomy, precision agricul- ture, detection of residual pesticides, fertilizers and tox- ins, and plant pathological monitoring (Fig. 1) (Rai et al. 2012). The innovation and designing of some nanosen- sors are correlated with the particular application in the respective area of the food and agriculture sectors. The commercializations of the presently designed nanosensors are crucial for the sustainable use of the technology, pos- sible after firm utilization of intellectual property right and patent rights.

This article is an abridged version of the chapter pub- lished by Srivastava et al. (2017).

Fig. 1 Schematics depicting the major nanostructures used in the area of food and agriculture sector. MNPs magnetic nanoparticles, AuNPs gold nanoparticles, upconversion nanoparticles, QDs quantum dots, SWNTs single-wall carbon nanotubes, MWNTs multiwall car- bon nanotubes, nanobarcode technology and electronic nose are the

major nanotechnological integrations utilized in the development of the suitable nanosensors or nanobiosensors. At present, a major appli- cation of nanosensor or nanobiosensor in the area of agriculture and food industries is inscribed

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Nanosensors and nanobiosensors: general design and principle

As mentioned previously, the biosensor operates on the basis of two principles; biological recognition and sensing. The prefix nano in the nanosensors and nanobiosensors is integrated after functionally transforming the sensing component with nanostructures for enhanced output. The crucial function of the cognition system is to provide spe- cific receptor for initial recognition and attachment with functional sensitivity. The transducer serves as a sensor fabricated with the nanomaterials such as metallic gold and iron oxide nanoparticle, quantum dots, graphene oxide and carbon nanotube. The nanoconfinement, flexible mor- phology, enhanced optical, mechanical, electrical, thermal properties, and high specific surface area of the nanomate- rial enhance the transducing capability to a certain degree. Nanosensors or nanobiosensors are categorized based on transduction mechanism for generation of output; as elec- trochemical nanosensors rely on the nanomaterial or CNT- based electrode; optical nanosensors are attributed with the enhanced optical property of the metallic nanoparticle, upconversion nanoparticle, and quantum dots. The third category of mass nanosensors with comparatively fewer implications in the area of food and agriculture sector relies on the mechanical and piezoelectric properties of

microcantilever and crystals, respectively, represented in the schematic in Fig. 2.

Electrochemical nanosensors

Electrochemical sensors are the most commonly used and widely accepted sensor functions on the principle of elec- trochemistry. The electron consumed or generated during biointeraction produces electrochemical signals, measured by electrochemical methodologies. The electrochemical nanosensors rely on chemical reactions between nanofab- ricated chemical, biomolecule, and the biological element and target analyte to produce or consume ions or electrons, measured as voltage, current, or impedance (Asha Chaubey 2002). The high sensitivity of electrochemical transducers, their compatibility with modern miniaturization/nanofabri- cation technologies, minimal power requirements, robust- ness, economical cost, low maintenance, rapidity, low detec- tion limits, and simplicity make it applicable for the sensing applications. The electrochemical signal generated quanti- tatively correlated with the amount of analyte present in a sample. Based on their working principle, electrochemical nanosensors device could be categorized in amperometry, voltammetry, and potentiometry.

The amperometric sensor is a variant of an electrochemi- cal sensor that continuously measures current generated due

Fig. 2 A typical nanobiosensor comprises of essential components starting from sample analyte to bioreceptor, transducer with inte- grated nanostructures, and finally detectors (left to right); analytes are chemical or biological entity which serves as a sample for quantita- tion or detection, which is unique to the bioreceptor. Bioreceptor is the recognition molecule of biological origin that could be the func- tional or structural protein, oligonucleotide including aptamers, com-

plete microbes or its component, cells, specific tissue and any subcel- lular organelle. The biological response is transferred to the detector via transducer integrated or functionalized with nanostructures, i.e., metal nanoparticles, magnetic nanoparticles, upconversion nanoparti- cle, quantum dots, carbon-based material such as graphene oxide and carbon nanotubes for enhanced detection via electrochemical, optical and mass detection methods. Here, NPs abbreviated for nanoparticles

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to the redox reaction of an electroactive species. The poten- tial is fixed at a constant value, and the Faradaic current is measured to determine the concentration of the electroactive species (Asha Chaubey 2002). The peak value of current observed over the linear voltage range shows the propor- tionality with the electroactive analytes. The real applica- tion of amperometric nanosensors initiated in the area of health care and diagnostic with the development of ATP sensor (Kueng et al. 2004), advance pregnancy test based on beta-HCG sensor (Santandreu et al. 1999). The nano- fabrication methodology makes amperometric biosensors more reliable, cheaper, and highly sensitive to expand the application from clinical to environmental, food and agricul- ture sector. Detection of organophosphates (Yan et al. 2013), sulfonamides (Xu et al. 2013), ractopamine and salbutamol (Lin et al. 2013), fructose content (Antiochia et al. 2013), hydrogen peroxide (Nasirizadeh et al. 2015) is the example of amperometric-based nanosensors and being discussed in detail in application section.

Voltammetry is a subsequent measurement of current by varying a potential in a controlled way. Cyclic voltamme- try is preferably used to get the redox potential and elec- trochemical reaction rates of the electrochemical reaction with analyte. The voltage parameter varies between the reference electrode and working electrode, by measuring the current between the working electrode and the counter electrode. The obtained data plotted as current versus volt- age are known as a voltammogram. The cyclic voltammetry has some applications in agriculture and food sectors like detection of carbosulfan in rice (Nesakumar et al. 2016), Salmonella typhi (Singh et al. 2015), heavy metal contami- nation in food sample (Yavuz et al. 2016).

Potentiometric sensors measure potential at working electrode with respect to the reference electrode. The output signal is generated because of accumulation of ion at ion- selective electrodes and ion-sensitive field effect transistors at equilibrium. ISE detects ions such as Na+, K+, Ca2+, H+, or NH4+ in complex biological matrices by sensing changes in electrode potential (Koncki et al. 2000). The implications of electrochemical nanosensor in the detection of various analytes such as preservatives, antibiotics, pesticide, and heavy metal in various food and agriculture are discussed in the later sections (Duran and Marcato 2013).

Optical nanosensors

Optical biosensors rely on the detection of the change in the optical signal made it highly compatible with various spec- troscopic measurements, such as absorption, fluorescence, phosphorescence, Raman, surface-enhanced Raman scat- tering, and refraction by detecting changes in wavelength, phase, time, intensity, and polarity of the light. In general, a

large variety of optical methods have been used in biosen- sors, based on fluorescence spectroscopy, surface Plasmon resonance, interferometry, and spectroscopy.

Luminescence comprises dual components: fluorescence and phosphorescence. The electron in the ground state excited by incident light leads to excited singlet electron in an excited state which upon returning to the ground state emits photons. Fluorescence-based nanosensing has owed high sensitivity, fast response, and ability to afford high spa- tial resolution through spectroscopic and imaging method- ologies. The implications of gold nanoparticles, silver nano- particles, and quantum dots possess the inherent property of fluorescence heavily depending on the size and morphology of the nanoparticle represented in Fig. 3B. Some instances such as detection of nitrite (Chen et al. 2016), reactive oxy- gen species (Hu et al. 2014), pathogenic bacteria such as S. aureus, V. parahemolyticus, and S. typhimurium, E. coli (Wu et al. 2014); detection of organophosphates have been done by fluorescence-based nanosensors (Dasary et al. 2008).

Quantum dots are the nanoclusters of few hundred to thousand atoms in the form of binary compound as CdSe, GaAs, InAs, SiC, CdTe and ternary compound of InGaN, InGaP, and InGaAs. Quantum dots show the inverse rela- tion between size and band gap; as the size of quantum dots increases, the band gap and emission wavelength decrease.

In the nanoconfinement, quantum dots exhibit full wavelength multicolored fluorescence with high quantum yield, longer fluorescence lifetime, enhanced photostabil- ity as well as an arrow emission spectrum. The size and band gap in the quantum dots are determinant of the emis- sion wavelength that gives a unique applicability to be used as a suitable fluorescent donor in fluorescent reso- nance energy transfer, FRET. The exceptional multiwave- length emission fluorescence, initiated with its application as a fluorescent label in the bioimaging and biomolecular assay with further progress on the application as quantum dots FRET-based examination of enzyme activity, track- ing intracellular gene delivery, single molecule detection and biophysical studies, detection of specific cellular and subcellular targets, multicolor barcodes, and imag- ing. Moreover, the innovation in the quantum dots-based sensing system progressed with selective functionalization of the quantum dots open the doors for the application of functionalized quantum dots agriculture and food industry. Recently, the CdSe and ZnS quantum dots are surfaces modified with the silane group and conjugated with the methylacrylate functionalized molecularly imprinted poly- mer to develop a quantum dots-based optosensor for detec- tion of dicyandiamide in the milk product. The concentra- tion of the dicyandiamide could be linearly correlated with the fluorescent quenching of the quantum dots (Liu et al. 2016). In another work highly sensitive and rapid response graphene quantum dots were prepared and developed as a

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resistive microsensor interdigitated electrode which selec- tively measures the soil moisture content by reading gravi- metric moisture content in the form of ionic conductivity (Kalita et al. 2016).

Surface plasmon resonance (SPR) is another domain of optical sensing utilized for highly sensitive and rapid detec- tion. The collective coherent oscillations of free electrons in the conduction band of metal are first excited by the interactive electromagnetic field at a metal/dielectric interface, and these created charge density oscillations are called surface plasmon polaritons (SPPs). The SPPs lead to the appearance of the elec- tric field that exponentially decays and diminished after pen- etrating few nanometer in surrounding matrix. As a result, the evanescent field is highly sensitive toward the refractive index change in the surrounding medium as depicted in Fig. 3C. Even small fluctuations in the refractive index of the medium alter the characteristics of the incident light beam such as wavelength, phase, and angle; and SPR excitation will change accordingly. Nanomaterials including metallic nanoparticles, magnetic nanoparticles, carbon-based nanostructures, latex nanoparticles, and liposome nanoparticles are engineered to show enhanced SPR sensing system for detecting concanavalin

A, antibiotics, mycotoxins, and pathogen like E. coli (Evtugyn et al. 2013; Huang et al. 2013; Zeng et al. 2014).

The amplification of the signals in surface-enhanced Raman scattering (SERS) arises by electromagnetic interaction of light with the metallic nanoparticle, which produces large amplifications of the laser field through excitations, known as plasmon resonances. Surface-enhanced Raman scattering is being a promising analytical technique that can be used to overcome problem related to a sensitivity of detection. When analyte molecules are deposited on the nanoparticle surface, their SERS signals are greatly increased at SERS-active sites known as “hot spots” because of electromagnetic and chemical enhancement effects shown in Fig. 3A. The detection sensitiv- ity increased up to 1014 orders of magnitude used for detection of antibiotics, pesticides such as malathion and sulfonamides (Dasary et al. 2008; Guillén et al. 2011).

Nanobarcode technology

Barcode technology follows the principle of symbology by interpreting the encoded data or information in the form of a map. Formally, “biobarcode” or “DNA barcode” technology

Fig. 3 Molecular process of optical detection comprises surface- enhanced Raman spectroscopy A showing principle construct of the sensing surface made up of gold nanostructure making the analyte highly sensitive to the Raman detection. In the typical detection pro- cess, a calibration curve is drawn after collecting and the Raman shift is positively correlated with the concentration of the analytes. Surface

plasmon resonance appears after differential absorbance of the metal NPs (gold NPs, silver NPs, QDs, and upconversion NPs) in different dispersion stages (B). The resulting changes occur after interactions with the respective analytes observed either in chromic/fluorescence shift or as fluorescence quenching of the native fluorescence (C). NP: nanoparticle, QD: quantum dot

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is novel tool extensively utilized for the identification of single species of animal, plant, microbes by taking a small stretch of a single gene (Ferri et al. 2009). The methodology includes a collection of short DNA sequences from different species and analysis of the data by constructing phylogenetic tree via distance-based neighbor-joining method. A 650-bp short sequence of mitochondrial cytochrome c oxidase subu- nit I gene abbreviated as COX-I or COI was extensively used for taxonomical identification of American birds, Australian fishes (Yancy et al. 2008), and tropical lepidopterans with the success rate of 98–100%. The recombinant DNA technol- ogy opens the door for construction of universal DNA-based barcode technology that enables the sample to analyze with one polymerase chain reaction-based sequencing by utiliz- ing universal primers. The non-coding nucleotide sequence is inserted in between the construct with common begin and end sequence in an orientation that recognized by universal primer in PCR to amplify the whole construct. The above construct could be transformed in the targeting organism to provide a tag for detection. The biobarcode constructed almost unaffected by frameshift mutation or any single-point mutation in PCR amplification (Gressel and Ehrlich 2002). Similar oligonucleotide index demonstrated as biobarcode with the PCR-based sequencing of 17 species of Scombridae family members frequently present in the processed sea food (Botti and Giuffra 2010). In the last decade, several biocide sensing applications have been developed such as monitor- ing physiological condition of Saccharomyces cerevisiae in the food processing and fermentation technology (Delneri 2010), identification of fish species (Arami et al. 2011; Asis et  al. 2016; Chang et  al. 2016; Handy et  al. 2011; Yang et al. 2012), discrimination between mixed meat specimen (Colombo et al. 2011), analysis of Lathyrus clymenum adul- terants (Ganopoulos et al. 2012), estimation of nematodes in flowerbed and agriculture soil (Morise et al. 2012), identifi- cation of food associated insect pests(Cho et al. 2013), food and vegetable safety and quality control observation(Jones et al. 2013; Maralit et al. 2013; Qiao et al. 2013). The recent development has been made by utilizing the nanotechnology with the use of metallic and magnetic nanoparticles in prac- tice. The dual gold nanoparticle and iron oxide nanoparticle have been separately conjugated with two different DNA barcodes for rapid and robust detection of Salmonella enteric Serovar Enteritidis in the food sample (Zhang et al. 2009).

e‑NOSE and e‑TONGUE

The electronic nose and electronic tongue are functionally analogous to the human sensory perception of odor and taste. The odor of volatile component and taste of nonvola- tile component keep crucial information about the quality and quantity of the material in food, beverages, agriculture,

pharmacology, personal care product manufacturing and processing (Baldwin et al. 2011). The e-nose and e-tongue are becoming the alternatives and substitute of the human sensory expert panel and consumer panel established for the quality assessment and quality control during the manu- facturing processes to fulfill maximum consumers satisfac- tion. e-nose comprises four components such as sampling headspace system, a sensor array, electronic data acquisi- tion control system, and a pattern recognition software. The sensor array composite of the chemical sensors which upon contact with the volatile analyte changes the conductance and gives a detection signal to the acquisition system. Metal oxide sensors, conductive polymer sensors, quartz crystal microbalance sensors, optical sensors, surface acoustic wave sensors, gas-sensitive field effect transistors are the major kind of sensors used as a component of an electronic nose (Martin et al. 2001). The metal oxide sensor array is prepared by depositing the thin layer of doped metal oxide on the ceramic or the high-temperature resistant plate. The concentration of dopant material determines the sensitivity and response time of the sensor to the analyte. Conductive polymer-based nanosensors are constructed by electrochem- ical deposition of conductive polymer precursor over the silicon substrate. The metal oxide sensor and conductive polymer-based sensors are the most common type of the sensor array used for the detection. The quartz crystal bal- ance is a coated resonator element that gives the response by changing the oscillation frequency after contact of the analyte (Di Natale et al. 1997). The data from the sensor array are being analyzed and classified by the subsequent electronic component by multivariate signal processing, which in turn processed by the pattern recognition software based on parametric and nonparametric algorithm such as principal component analysis (PCA), linear discriminate analysis (LDA), partial least squares (PLS), functional dis- criminate analysis (FDA), cluster analysis (CA), fuzzy logic or artificial neural network (ANN), and probabilistic neural network (PNN) analysis (Scott et al. 2006). e-tongue is com- plementary in the principle of detection and post analysis. The major two differences are: The first is in the selectivity of the liquid sample, and second, it gives the result output in the form of saltiness, bitterness, sweetness, sourness, and metallic taste (Fig. 4). The compound having higher vapor pressure and low boiling points is small molecular weight (< 350 Da) organic compounds with several polar and non- polar groups which are highly volatile called volatile organic compounds (VOCs). The VOCs like pyruvic acid, glypho- sate, acetic acid and citrinin are specifically present in the plant cell, pesticides, microbes, and food product, respec- tively (Wilson and Baietto 2009). The selectivity, sensitiv- ity, redundancy, accuracy of the sensors, response time, and reliability of the e-nose and e-tongue make it most suitable device for the sensing application in agriculture, forestry,

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and food industry. The VOCs release from the food com- ponents are making the e-nose and e-tongue more appli- cable in area of food technology from monitoring of raw and manufactured product, cooking and fermentation pro- cess, product packaging, storage and quality assessment for long-term storage (Concina et al. 2012; Peris and Escuder- Gilabert 2013). Recently, the e-nose and e-tongue have been used for the evaluation of aroma transfer from food plastics bags (Torri and Piochi 2016), quality assessment of beef fillets (Mohareb et al. 2016), detection of Alicyclobacillus acidoterrestris spawned spoilage in apple juice (Huang et al. 2015), detection of mixed edible oil (Men et al. 2014), and identification of adulterated milk (Yu et al. 2007).

Wireless nanosensors and wireless sensor network

A wireless sensor network abbreviated as WSN is self- organizing with intelligent decision-making capability, self-dynamic topological configuration, self-diagnostics with context awareness and fault tolerance, and self-heal- ing autonomous operating mode with information security system made up of several components of radio-frequency transceivers, sensors or nanosensors node, microcontrollers, and power sources. The microelectromechanical and

nanoelectromechanical system-based sensors node mini- mized the cost, size, and power consumption and gave a reli- able measurement of small change in pressure, temperature, humidity along with the temporal observation like proximity, position, speed, acceleration, and vibration at the place of observation. The limitless sensor flexibility and enhanced network robustness give enormous applications in environ- ment, defense, agriculture, and food industries.

Precision agriculture term is used for the agriculture practices with the integrated information and wireless con- trol technology in the farming or forestry. The agronomical inputs such as fertilizers and irrigation are being applied very precisely controlled by the crop growth response in a spatiotemporal manner. In practice, the wireless sensors net- work uniformly deployed in the soil collects and relays the soil information to the control central via sensors nodes. The control server analyzes and precisely decides the particular place where irrigation or fertilizer is required (Sahota et al. 2011). The design and deployment of the wireless sensors network are continuously expanding with multiple monitor- ing and control. A wireless sensor network-based irrigation management system WiPAM has been deployed, which fol- lows the workflow of taking soil moisture and temperature information at certain time interval, relaying and saving data in coordinator node, forwarding the data to remote monitor- ing system via a gateway node, and response value stored

Fig. 4 Typical electronic nose with its component; sample head space, nanosensor array, unit for algorithmic processing, and clas- sified data after the detection in form of a map. In the functional aspects, volatile organic compound from the specific sample source

of food, fruits and vegetables, microbes, pesticides, plant compo- nents, and waste reach to sensory array from sample head space. After sensory multivariate algorithmic processing, the signal is for- warded to pattern recognition software for mapping and result output

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in coordinator node directs the opening or closing of the irrigation valve. The whole workflow utilizes the several components such as wireless network, moisture and tem- perature sensors, coordinator node, gateway node, and auto- mated irrigation valve. ZigBee IEEE 802.15.4 is a low-cost and low-power-consuming personal area networking pro- tocol used for the wireless sensor networking. The sensors are deployed in the 40 cm in the deep soil around the root zone of the plant to sense the water potential, soil moisture potential, and temperature. The irrigation system comprises solenoid valves with optocouplers and switching transistors to control the on/off of the valves. Self-sustained irrigation management system collects the information at very 30 min and relays and makes the automated irrigation response (Mafuta et al. 2013). In addition to irrigation management system, the wireless sensor technology is being deployed for many application such as sensing leaf wetness and leaf area index in the agriculture field (El Maazouzi et al. 2014; Shimojo et  al. 2013), precise green house management (ArunKumar and Alagumeenaakshi 2014), in mango and black pepper farming (Kodali et al. 2013; Li et al. 2013). Moreover, some instances of application of wireless sensing network in the food industries are real-time traceability and food chain management system (Ko et al. 2014; Wang et al. 2015), under water wireless sensor network for marine fish farming and sustainability monitoring (Lloret et al. 2015).

Application of nanosensors and nanobiosensors in food sector

Detection of preservative food contaminant

The distinct shape- and size-dependent properties of metallic nanoparticles offer enormous potential applications in the area of food technology. The desirable optical, mechanical, chemical, antimicrobial and electronic properties of metallic nanoparticle make it novel for conjugation with enzymes, antibodies, ligands, drugs, colorimetric and fluorimetric agents, and other biomolecules, thus opening the way for sensitive diagnostic assays, radiotherapy, thermal ablation, gene and drug delivery, optical imaging, labeling of biologi- cal systems, effective antimicrobial activities, and detoxifi- cation of hazardous compounds (O’Neal et al. 2004). Addi- tionally, metallic NPs have a huge role in food production, packaging, consumption, ability to quick response against pathogens, pesticides, and other toxic residues through detection of microbial deterioration of food quality and con- taminant. Among the metallic nanoparticles, the colloidal gold nanoparticle has been mostly applied for various appli- cations because of the flexible size range of sub-10–250 nm and complex shape-dependent optical and mechanical prop- erties (Castro et al. 1990).

In the context of optical property, the extinction spectra of gold nanoparticles are dominated by localized surface plasmon resonance, as coherent excitation of the conduction band electrons by oscillating electromagnetic field induces coherent oscillation on the positive metallic lattice. The incorporation and aggregation of gold nanoparticle parti- cles on nanosensor platform greatly enhance the sensitivity of localized surface plasmon resonance by 2–10-folds and surface-enhanced Raman scattering by 106–109-fold (Jain et al. 2007). The strong local surface plasmon resonance absorption with extremely high extinction coefficients in the visible wavelength range is the characteristics of gold nanoparticle and gives a color transition from wine red being in dispersion state to blue after attaining aggregation state. The estimation of the residual amount of antibiotics in milk, dairy product, and meat is one of the demanding prospects in food technology. The gold nanoparticle synthesized using pyrocatechol violet as a reducing agent in such a way that it gives surface hydroxyl group functionality could be linked with hydroxyl and amide group of the antibiotic via hydro- gen bonding. The quantity of antibiotics like kanamycin, neomycin, streptomycin, and bleomycin could be detected by general color change even with the less concentration of 1 × 10−9 M. Alternately, with advancement in approach the sensitivity of detection is enhanced by functionalizing gold nanoparticles with thioaniline and mercaptophenyl boronic acid. Here thioaniline serves as an electropolymerized agent, whereas mercaptophenyl boronic acid provides the pH- dependent reversible binding capability, stabilizes the com- plex and prevents from precipitation. The thioaniline cross- linked gold nanoparticles composites create a molecularly imprinted matrix comprising high sensitivities toward the sensing of the antibiotic analytes. The quantity of neomycin, kanamycin, and streptomycin is detected by analyzing the surface plasmon resonance curve before and after imprinting with the sensitivity of 2.00 ± 0.21 pM, 1.00 ± 0.10 pM, and 200 ± 30 fM, respectively (Frasconi et al. 2010).

The carcinogenic nitrile pollutant was detected using silver nanoparticle-based nanosensor comprising hyper- branched polyethyleneimine. The reaction of nitrite with hydrogen peroxide generates peroxynitrous acid under acidic conditions and induces the aggregation of silver nanoparti- cle, and fluorescence quenching has been correlated with the concentration of nitrite within the limit of detection of 100 nM (Chen et al. 2016).

Gold nanoparticles enhanced surface plasmon reso- nance used for detection of ochratoxin A is a mycotoxin produced by Aspergillus and Penicillium species often agri- food contaminant. Thiolated aptamer sequences specific to ochratoxin A are covalently attached to gold nanopar- ticles via Au–S bond for detection of ochratoxin A toxin (Evtugyn et al. 2013). The sensing mechanism is based on the ability of antioxidants to protect the fluorescence of gold

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nanoparticles, and method is used for evaluating the anti- oxidant content in commercial fruit juices and proves to be superior to existing spectroscopic sensing methods regarding rapid response, ease of use, and good biocompatibility (Hu et al. 2014).

The contamination of natural honey with residues of sul- fonamides is a major concern to food companies, and these residues of antibacterial drugs in honey give toxicological risks and allergenic effects. In the approach, polyclonal anti- serum against sulfathiazole conjugated with colloidal gold nanoparticles serves as detection reagent for lateral flow immunochromatographic assay (Fig. 5). This device for the detection of sulfathiazole is a cost-efficient and portable sin- gle-antigen directed immunoassay. The device constructed on a plastic support with over-mounting of nitrocellulose membrane of thickness 15  ±  1  µm. Protein hapten-con- jugated OVA-S2 attached at the “test line,” whereas goat antirabbit antibody at “control line” position. Dispensing gold nanoparticles conjugated with purified sulfathiazole antiserum onto sample port “S” of the device leads to rapid

wet through of the conjugate pad, solubilizes the gold-con- jugated antiserum. The gold nanoparticle conjugated from conjugation pad migrates down to the nitrocellulose mem- brane by capillary action. Control experiments made with buffer or honey without sulfathiazole display two red lines as “C” line and the test area “T” line indicating a negative assay, whereas honey samples containing sulfathiazole yield a bright red line at the control area “C” line without any change at the test line “T” line showing the positive test. The intensity of the test line is inversely correlated with the concentration of sulfathiazole present in the sample. The developed assay is showing a fascinating rapid detection nanobiosensor with a limit of detection of 10 ng and detec- tion time of 10 min (Guillén et al. 2011).

The nanofunctionalization approach gives the flexibility to coat the desirable analyte over the such as a glassy carbon electrode modified with gold nanoparticle sand used for the quantitation and sensing of butylated hydroxyanisole, butyl- ated hydroxytoluene, and butylated hydroquinone by linear sweep voltammetry with detection limit of 0.039, 0.080, and

Fig. 5 Lateral flow immunochromatographic assay (LFIA) is used for the detection of sulfonamides as a contaminant in the honey sample. The single-antigen directed immunoassay-based device constructed on nitrocellulose membrane of 15 µm, the protein hapten-conjugated OVA-S2 was printed at test line “T,” while goat antirabbit antibody at control line “C”, the excess of gold-conjugate antiserum is trapped by goat antirabbit (GAR) immunoglobulins displaying the control line C

through the Fab region (heavy chain of immunoglobulin molecule); the gold nanoparticle conjugated sulfathiazole antiserum is adsorbed on the conjugate pad. The sample containing sulfathiazole after pass- ing through sample pad binds with the conjugates in conjugate pad and shows only red color on “C” line, whereas control without sam- ple passes through conjugate pad and develops red color at both the “C” and “T” line, respectively

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0.079 gm L−1, respectively (Lin et al. 2013). Zearalenone is an estrogenic mycotoxin produced by Fusarium species and induces the accumulation of high levels of estrogen in animals and hampers reproductive system functions. Strepta- vidin–HRP–gold nanoparticles-based chemiluminescence immunoassay is developed for sensitive detection (Wang et al. 2013).

In other approaches, xanthine oxidase enzyme specific to xanthine was immobilized covalently onto chitosan-bound gold-coated iron nanoparticles, electrodeposited on pencil graphite electrode surface to serve as a working electrode. Using Ag/AgCl as reference and Pt as auxiliary electrode electrochemical detection of the xanthine has been done with the limit of detection of 0.1 µM (Devi et al. 2013).

Aflatoxin M1, a hydroxylated metabolite of aflatoxin B1, is often found in milk from animals fed with aflatoxin B1-contaminated feeds, and several qualitative and quantita- tive methods have been developed to detect aflatoxin M1 in milk and other dairy products. In the approach, gold nano- particles-labeled aflatoxin M1 conjugate, bovine serum albu- min with surface lysine residues, and the anti-AFM antibody were linked on the surface of magnetic beads by the oriented coupling effect of recombinant protein G. Post-incubation, separation by the magnetic beads and dynamic light scatter- ing analysis shows that the intensity of nanoprobe in bulk solution is positively proportional to the concentration of Aflatoxin M1 in a sample solution with the lower possible measurement limit of 27.5 ng L−1 (Zhang et al. 2013). Based on the same principle, a sensitive and rapid immunodipstick colloidal gold antibody probe is developed for the detection of vitamin B12 in various food samples. The color intensity developed was inversely proportional to the vitamin B12 concentration with detection limit of 1 ng mL−1(Selvakumar et al. 2013).

Carbon nanotubes exhibit the enormous potential for development of nanosensors and nanobiosensors for uncountable applications and revolutionize the area of nanobiosensor technology with properties such as tiny size, high strength, high electrical and thermal conductivity, and high specific surface area (Lijima 1991). Quinoxaline- 2-carboxylic acid is the marker residues of carbadox, which is a constituent of food as additives in pork, chicken, and fishes having strong mutagenic and carcinogenic effects (Čihák and Vontorkov 1983). Consequently, approach to detect the trace level of quinoxaline-2-carboxylic acid, mul- tiwalled carbon nanotubes is functionalized with chitosan fabricated on glassy carbon electrode. Sol–gel molecularly imprinted polymer film serves as a recognition element (Tkac et al. 2007). The constructed electrode demonstrated as a reproducible and reliable electrochemical sensor for accurate quantification of quinoxaline-2-carboxylic acid at trace levels in meat samples with a low detection limit of 4.4 × 10−7 mol L−1(Yang et al. 2013b).

In another approach, single-walled carbon nanotube has been used for detection of d-fructose in fruit juices, honey, soft and energy drinks (Stredansky et al. 1999). An immo- bilized fructose dehydrogenase enzyme-based biosensor developed by using osmium redox polymer as redox media- tor shuttles the electrons between the immobilized fructose dehydrogenase enzyme and the single-walled carbon nano- tube pasted on the working electrode. The optimized bio- sensor required only five units of enzyme and kept the 80% of its initial sensitivity after 4 months. The biosensor has a detection limit for fructose to estimate 1 µM with a high sen- sitivity, good reproducibility, and a fast response time of 4 s (Antiochia et al. 2013). Additionally, carcinogenic Sudan I is detected by multiwall carbon nanotube thin film-modified electrode. Enhancement of electrochemical oxidation on the electrode surface by Sudan I dye was determined by an elec- trochemical method with the limit of detection 5.0 µg L−1 (Gan et al. 2008).

Detection of food‑borne pathogens and microbial load

The presence of pathogenic microorganisms in the food- stuff is the serious concern of food industry. The failure or minor delay in the detection of contaminating pathogen leads to spoiling of the food and fatal health issues. The real-time detection of the pathogen is a prerequisite for food safety and quality management. The recent advancement in the sensing technology provided a platform to detect some microbial contamination, chemicals, and toxins in specific, sensitive and in less time. The food-borne pathogen species such as Campylobacterspp, Salmonellaspp, Listeriamono- cytogenes, and Escherichia coli O157:H7 have been found to be responsible for the majority of food-borne outbreaks (Velusamy et al. 2010). Here in this section, we are elaborat- ing the nanosensors- and nanobiosensors-based approaches to detect some pathogens in real food samples which are listed in Table 1.

Brucellosis is a global zoonotic infectious disease caused by Brucella spp. in cattle spread either by consumption of unpasteurized dairy products or by direct contact with afflicted animals. Antigen-tagged fluorescent silica nano- probes are utilized to detect Brucella IgG antibodies in milk samples of afflicted animals. The sensing is accurate and repeatable, with high specificity and sensitivity and requires a small amount of sample, i.e., 50 µL within short duration of 10 min (Vyas et al. 2015). In another approach, Liposome-amplified plasmonic immunoassay is overcoming the requirement of sophisticated spectroscopic and imaging instrument and protocol. This method is ELISA-inspired detection approaches even though the limit of detection ranging from the femtomolar (10−15 M) to attomolar (10−18 M). The dependency of the optical property of plasmonic

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nanostructures on their size, shape, distribution, and com- position has been exploited here to demonstrate an enzyme- less, naked-eye detection of a single-digit pathogen using plasmonic colorimetry of gold nanoparticles combined with signal amplification via cysteine-loaded liposomes. The

immunocomplex is directly labeled with cysteine-loaded nanoliposomes using a biotin–streptavidin linkage. Gold nanoparticle solution is then added to the assay, followed by the addition of a hydrolytic agent. In the presence of a pathogen, the surfactant induces immediate hydrolysis of

Table 1 Various pathogens and contaminant interferes with production, processing, and storage and quality of the food products

The table represents the detection application, nanomaterial used for the construction of nanosensor, mode of detection, the limit of detection, and the references (left to right) AuNPs gold nanoparticle, DLS dynamic light scattering, GCE glassy carbon electrode, and UCNPs upconversion nanoparticles

Target element Nanomaterial Detection method Limit of detection References

Pathogens  Listeria monocytogenes and

Salmonella enterica Thiol–gold NPs–PCR product Colorimetric 0.015 and 0.013 ng mL−1 Devi et al. (2013); Fu et al.

(2013)  Brucella spp Fluorescent–silica nanoparticle Fluorescence 50µL Vyas et al. (2015)  E. coli,  Salmonella spp, and  Listeria

Cysteine-loaded nanoli- posomes

and AuNPs

Liposome-amplified plasmonic immunoassay (LAPIA)

6.7 attomolar Bui et al. (2015)

 S. aureus, V. parahemolyticus, S. typh-

imurium

Multicolor UCNPs–MNPs– aptamers

Luminescence bioassay 25 CFU mL−1 10 CFU mL−1 15 CFU mL−1

Wu et al. (2014)

 Escherichia coli O157:H7 Fluorescent–silica nanopar- ticles

Fluorescence 1000 times Zhao et al. (2004)

S. typhimurium AuNPs–GBP-ProA protein Surface plasmon resonance (spr) immunosensors

10 fold Ko et al. (2009)

 Escherichia coli O157:H7 and Enterobacter sakazakii

Multiwalled carbon nanotubes (MWCNTs)/sodium alginate (SA)/carboxymethyl chitosan composite films

Electrochemical immunosen- sor

4.57 × 103 CFU mL−1 and 3.27 × 103 CFU mL−1

Dou et al. (2013)

 Salmonella paratyphi A Single-walled carbon nanotubes (SWNTs) and DNAzyme–Apt22

Chemiluminescence 103 CFU mL−1 Yang et al. (2013a)

Food contaminants  Kanamycin mono sul-

fate, neomycin sulfate, streptomycin sulfate, and bleomycin sulfate

AuNPs Strong local surface plasmon resonance

1 × 10−9 M Zhang et al. (2013)

 Neomycin, kanamycin, and streptomycin

Bis-aniline–cross-linked Au NP

Surface plasmon resonance 2.00 ± 0.21 pM, 1.00 ± 0.10 pM, and 200 ± 30 fM

Frasconi et al. (2010)

 Nitrite Hyperbranched polyethyl- eneimine scaffolds–AgNPs

Fluorescence quenching 100 nM Chen et al. (2016)

 Ochratoxin A Au nanoparticles Enhanced SPR 60 pg mL−1 Evtugyn et al. (2013)  Quinoxaline-2-carboxylic

acid MIP/sol–gel/MWNTs–CS/

GCE Electrochemical detection 4.4 × 10−7 mol L−1 Yang et al. (2013b)

 d-fructose FDH–single-walled carbon nanotube paste electrode

Electrochemical detection 1 µM Antiochia et al. (2013)

 Sudan I Multiwall carbon nanotube thin film-modified electrode

Electrochemical detection 5.0 µg L−1 (Gan et al. 2008)

 Butylated hydroxyanisole, butylated hydroxytoluene, and butylated hydroquinone

AuNPs/GCE Linear sweep voltammetry 0.039, 0.080 and 0.079 µg mL−1

Lin et al. (2013a, b)

 Sulfathiazole OVA–hapten conjugate and AuNPs

Lateral flow immunoassay 15 ng g−1 Guillén et al. (2011)

 hROS AuNPs Fluorescence–logic gate integration

5 µM Hu et al. (2014)

 Xanthine XOD/CHIT/Fe-NPs@Au/PGE Electrochemical detection 0.1 µM Devi et al. (2013)  Aflatoxin M1 DLS–superparamagnetic

beads–AuNPs Dynamic light scattering 37.7 ng L−1

in buffer solution and Zhang et al. (2013)

 Vitamin B12 AuNPs Immunodipstick 1 ng mL−1 Selvakumar et al. (2013)

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the liposomes and releases encapsulated cysteine molecules. Due to their high affinity to the gold surface, the thiol groups of cysteine will bind to the nanoparticles, while the free amine and carboxyl groups bind to other cysteine molecules via intermolecular hydrogen bonding inducing rapid aggre- gation of a gold nanoparticle. Since assembled nanoparticles exhibit light absorbance at higher wavelengths, the aggrega- tion is reflected by a rapid and highly distinctive color shift of the solution from red (650 nm) to dark blue (520 nm), which allows naked-eye assessment. This assay has been done to confirm the presence of E. coli, Salmonella, and Listeria in milk, ground beef, and apple juice with the limit of detection of 6.7 attomolar (Bui et al. 2015).

Alternatively, luminescence bioassay was demonstrated for simultaneous detection of three food-borne pathogenic bacteria utilizing three types of PAA-modified NaYF4: Yb,Tm multicolor upconversion nanoparticles served as sig- nal probes, with independent fluorescence emission peaks. These multicolor upconversion nanoparticles conjugated with the amino-modified aptamers specific to S. aureus, V. parahaemolyticus, and S. typhimurium developed by condensation reaction. Moreover, magnetic nanoparticles were conjugated with cDNA complementary to individual aptamers. Aptamer and cDNA hybridization leads to the formation of a complex of upconversion nanoparticles and magnetic nanoparticles, as signal probe shows maximum luminescence at 477 nm as a negative control in the absence of bacteria. The subsequent reduction in the fluorescence on the addition of bacteria is correlated with the bacterial load. This biosensing strategy is utilizing multicolor upconversion nanoparticles in conjunction with magnetic nanoparticle and aptamers as analytical methods for detection of pathogenic bacteria S. aureus, V. parahemolyticus, and S. typhimurium in the minimum count of 25, 10, and 15 CFU mL−1 (Wu et al. 2014).

The colloidal gold nanoparticles directly assembled onto a surface of the gold chip with 2-aminoethanethiol give a sensitive label-free detection system. A novel fusion protein was constructed by genetically fusing gold binding polypep- tides to protein A as a cross-linker for efficient immobiliza- tion of antibodies. The GBP-ProA protein directly immo- bilized onto both bare and gold nanoparticle assembled on surface plasmon resonance sensor chip surfaces via the GBP portion, followed by oriented binding of the antibody. This signal enhancement in the gold nanoparticle assembled chip causes a tenfold increase in detection of S. typhimurium compared to the bare one (Ko et al. 2009). Escherichia coli O157:H7 is one of the important agents of food-borne dis- eases. Therefore, a simple, quick, and precise detection of E. coli O157:H7 is crucial for minimizing or eliminating potential infections. In this particular sensing technique, fluorescent Tris(2,2-bipyridyl) dichlororuthenium(II) hexa- hydrate dye-doped silica nanoparticles are used for detection

of E. coli showing 1000 times enhanced fluorescence signal in comparison with pure dye. This approach is connected with the fact that each mesoporous silica nanovesicle can encapsulate thousands of organic dye molecules and capable of tagging the bacterium (Zhao et al. 2004).

Gold nanoparticles used for sensitive colorimetric detec- tion of two food-borne pathogenic bacteria: Listeria mono- cytogenes and Salmonella entericusing polymerase chain reaction-based amplification of bacterial genes to directly distinguish by naked eyes. The thiol-labeled PCR primer gives PCR products with thiol label, which upon mixing with unmodified gold nanoparticles solution results in the formation of gold nanoparticle–PCR products, showing that the target pathogenic bacteria sample could be specifically recognized and detected (Fu et al. 2013). Alternatively, in another approach, polyclonal antibody-coated colloidal gold particles used to develop a rapid and sensitive sand- wich immunochromatographic assay-based device can detect staphylococcal enterotoxin B contamination in food sample with the limit of detection of 1 ng mL−1 within duration of 5 min (Rong-Hwa et al. 2010).

Salmonellosis with the symptom of paratyphoid a fever is one of the most frequently reported bacterial food-borne illnesses (Maskey et al. 2006). The rapid and reliable method to overcome the laboratory-based culture detection method imposed by non-covalent self-assembly of single-walled carbon nanotubes and DNAzyme-labeled aptamer as detec- tion probes. Aptamer Apt22 with the lowest Kd value of 47  ±  3  nM is developed by an iterative approach called systematic evolution of ligands by exponential enrichment (SELEX). Carbon nanotubes possess the ability to protect ssDNA by π-stacking interactions between the nucleotide bases (Tuerk and Gold 1990). Binding of P0 with SWNT gives a stable P0/SWNTs complex and interferes with the formation of free hemin-containing active DNAzyme, and the system does not generate any detection signals. Addition of the target bacteria and hemin will specifically bind to the probe and compete with the individual SWNTs, tends P0 to be away from SWNTs, and leads to formation of hemin/G- quadruplex horseradish peroxidase-mimicking DNAzyme which in turn acts as a catalyst for the generation of chemi- luminescence (λ = 420 nm) through the oxidation of luminol by H2O2 with detection limit of 10

3 CFU mL−1 (Yang et al. 2013a).

An electrochemical immunosensor was constructed to detect the two pathogenic bacteria E. coli O157:H7 and Enterobacter sakazakii. The fabrication of the sensor was done by screen-printed carbon arrays constituting four carbon working electrode, an integrated carbon counter electrodes, and an integrated Ag/AgCl reference electrode. Multiwalled carbon nanotubes/sodium alginate/carboxym- ethyl chitosan composite films were coated on all the work- ing electrodes to enhance the sensitization of the electrode.

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Horseradish peroxidases-labeled antibodies of two bacteria were immobilized on the different working electrode. The results demonstrate the LOD of 4.57 × 103 CFU mL−1 and 3.27 × 103 CFU mL−1 for E. coli O157:H7 and E. sakazakii, respectively (Dou et al. 2013).

Application of nanosensors and nanobiosensors in agriculture

The long-standing application of nanosensors and nanobio- sensors is to estimate the presence and concentration of toxic chemicals in soil and wastewater. The net land contaminant

such as pesticides, herbicides, heavy metals and residues of fertilizers is accumulating and causing a decline in the resources and agricultural productivity. As discussed in the previous sections, nanomaterials are being used in the area of nanosensing and new strategies are revolutionizing the agriculture and food sector. The nanosensors are being used for quantitative and qualitative suitability of the farm- ing soil in the context of soil fertility and microorganism present. Among the plethora of nanosensors and nanobio- sensors in agriculture (Table 2), few are being elaborated in the framework of the utilized nanostructure. Here, the colloidal gold nanoparticles of 40 nm size are conjugated with the micron-sized polymer by modifying the surface

Table 2 Various contaminants such as residual pesticides and heavy metal ion interferes with soil fertility, crop production and harvesting, pro- cessing, storage, and quality of the agriculture products

The table represents the detection application, nanomaterial used for the construction of nanosensor, mode of detection, the limit of detection, and the references (left to right) AuNPs gold nanoparticles, GCE glassy carbon electrode, AchE acetylcholinesterase, SPR surface plasmon resonance, MWNT multiwalled carbon nanotubes, and GO graphene oxides

Target element Nanomaterial Detection method Limit of detection References

Malathion Aptamer–polymeric micro- sphere–AuNPs

SERS 3.3 µg mL−1 Barahona et al. (2013)

Chlorpyrifos and carbo- furan

AChE/L-cys/HGNs/Chits/ GCE

Electrochemical 0.06 µg dm−3 and 0.08 µg dm−3

Sun et al. (2013)

Carbofuran and triazophos Lateral flow immunochro- matographic

Optical 32 µg L−1 and 4 µg L−1 Guo et al. (2009)

Pinacolyl methylphospho- nate, methylphosphonic acid, glyphosate

Eu(III)-AuNPs Surface-enhanced fluores- cence

1 µmol dm−3 Dasary et al. (2008)

N-methyl carbamate AChE–AuNPs SPR 7 pM and 12 pM Huang et al. (2009) Parathion ZrO2/Au nanocomposite Square wave voltammetry 3 ng mL−1 Wang and Li (2008) Methyl parathion AChE/F–ZnSe/GR–Chi/

GCE Chronoamperometry 0.2 nM Dong et al. (2013)

Methyl parathion BSA–CdTe Bioconjugate Fluoroimmunoassay 0.1 ng mL−1 Chouhan et al. (2010) Deltamethrin CdTe–SiO2–MIPs Fluorescence quenching 0.16 µg mL−1 Ge et al. (2011) Paraxon AChE/CNT–NH2/GC

electrode Electrochemical 0.08 nM Yu, et al. (2015)

Mg2+, Ca2+, Sr2+, Ba2+ bis-aniline-bridged AuNPs composites

SPR Femtomolar Ben-Amram et al. (2012)

Concanavalin A GO/DexP–AuNPs SPR 0.39 μg mL−1 Huang et al. (2013) Dichlorvos MWCNTs/ALB)n/GCE Electrochemical 0.68 ± 0.076 µg L−1 Yan et al. (2013) Acetamiprid Aptamer–AuNPs Optical 0.1 ppm Weerathunge et al. (2014) Acetamiprid AuNPs–multiwall carbon

nanotube-reduced gra- phene oxide nanoribbon composites

Impedimetric 1.7 × 10−14 mol dm−3 Jampilek and Kral’ova (2015)

Malathion, chlorpyrifos, monocrotophos and carbofuran

AChE/Chit–PB–MWNTs– HGNs/Au

Electrochemical Nanomolar range Zhai et al. (2013)

Br− MWNTs–chitosan–GCE Electrochemical 9.6 × 10−8 µg mL−1 Zeng et al. (2005) Carbofuran Multiwall carbon nano-

tubes–graphene sheets– ethyleneimine polymer– Au nanocomposites

Electrochemical Immuno- assay

0.03 ng mL−1 Zhu et al. (2013)

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with 2-aminoethanthiol. The aptamer specific to malathion was thiolated at the terminal and attached to the gold nano- particle surface by thiol–gold chemistry. The micron-sized aptamer containing gold nanoparticle serves as an apta- sensing microsphere, specifically interacting and binding with the malathion and being detected by surface-enhanced Raman spectroscopy with the sensitivity of detection of 3.3 µg mL−1 (Barahona et al. 2013).

In another work, the hollow 50-nm gold nanoparticles were being synthesized and surface functionalized with l-cysteine. The cysteine assembles the chitosan electrostati- cally on the surface of hollow gold nanoparticle through Au–S chemistry. Moreover, the whole conjugated are deposited on a glassy carbon electrode. The assembly of enzyme acetylcholinesterase over the hollow gold nanopar- ticle is the crucial step in the process, which is covalently attached to the hollow gold nanoparticle surface via –COOH group incorporated by l-cysteine. The nanobiosensor con- structed by the subsequent assembly on working electrode and the immobilized enzyme AChE interact with the sub- strate acetylthiocholine chloride to produce the electroac- tive compound thiocholine, and the inhibition of the enzyme was measured by the oxidation current of thiocholine in the presence of chlorpyrifos and carbofuran. Linear relation- ships between inhibition percentage and the concentration of chlorpyrifos and carbofuran were used for quantitation with the detection limits of 0.06 µg dm−3 for chlorpyrifos and 0.08 µg dm−3 for carbofuran. The chlorpyrifos and car- bofuran are organophosphate and carbamate insecticide used in the agriculture field, and the monitoring of trace amount of above pesticide is crucial for public health and security (Sun et al. 2013). The strategy represents the morphological change in the gold nanoparticle to hollow gold nanoparti- cle which could significantly improve electron transfer and decrease the over-potential of substrate oxidation better than other biosensors.

The gold nanoparticles-labeled antibody-based lateral flow immunochromatographic was constructed for simulta- neous detection of pesticides as carbofuran and triazophos. Bispecific monoclonal antibody specific to both the pesti- cides imprinted on one nitrocellulose strip is parallel to this gold-labeled monospecific monoclonal antibody specific to carbofuran and triazophos separately immobilized on con- jugate pads of the another strip. The presence of carbofuran and triazophos can be visualized even in less concentration of 32 and 4 µg L−1, respectively, representing the method for rapid identification and quantification of pesticide as a contaminant (Guo et al. 2009).

The surface-enhanced fluorescence obtained near the nanostructured metal is concentrating effect of the incident light into local electromagnetic “hot spots,” on the surface of fluorophores; alternatively, metal nanostructures could alter radiative and non-radiative decay rates ultimately

changing both fluorescence lifetime and quantum yield. In the strategy gold nanoparticle-based surface-enhanced fluorescence spectroscopy for quick screening of organo- phosphorus agents such as pinacolyl methylphosphonate, methylphosphonic acid, glyphosate were observed with high sensitivity of 1 µmol dm−3. The Eu(III) ions within the proximity of gold nanoparticle experience strong elec- tromagnetic field and produce large fluorescence enhance- ment natively, but organophosphates preferably bind with Eu(III) ions induce dissociation from gold nanoparticle surface altered the fluorescence intensity which is corre- lated with the quantity of organophosphates (Dasary et al. 2008).

While increasing sensitivity and accessibility of the metallic nanoparticle, here single detection platform has been used for detection of more than one substitute of the single pesticide. The N-methyl carbamate as insecticides tar- gets AChE, even though it is widely used agriculture. Here two carbamate inhibitors with different ether linkages and the terminal lipoate were synthesized and labeled with gold nanoparticles, and specific interactions between the gold nanoparticle labeled carbamate inhibitors such as ALC1 and ALC2 were immobilized AChE on sensor chip surface by surface plasmon resonance with the possible limit of detection of 7 and 12 pM (Huang et al. 2009). Alternatively, zirconium oxide nanoparticle having a high affinity toward the phosphate group on organophosphate provides a basis for construction of ZrO2/Au nanocomposite film electrode, which can measure the presence of parathion with a limit of detection of 3 ng mL−1 by square wave voltammetry (Wang and Li 2008).

Quantum dots are nanocrystals with the unique property of high photostability, full wavelength absorbance, fluores- cence spectra, and controlled fluorescence emission. These properties of QDs are making it useful for the sensing and imaging applications (Ruedas-Rama et al. 2011). The ace- tylcholinesterase with mercaptophenyl boronic acid-func- tionalized ZnSe quantum dots electrostatically adhered on graphene–chitosan nanocomposites cast on a glassy carbon electrode were used for the quantitative electrochemical detection of methyl parathion with the limit of detection of 0.2 nM. Here, mercaptophenyl boronic acid derivatives have been used for its inherent capability to recognize cis- diol configuration in saccharides and to form a covalent bond via the formation of cyclic esters and used here for the fabrication purpose. The AChE/F–ZnSe/GR–Chi/GCE was constructed and used to detect methyl parathion by chronoamperometric measurement in the presence of ATCl substrate before after inhibition with methyl parathion of different concentrations. The observed oxidation current variation could easily correlate with the concentration of methyl parathion. This method introduced improved elec- tron transfer rate on the electrode interface with enhanced

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immobilization of enzyme for methyl parathion detection (Dong et al. 2013).

Moreover, intrinsic fluorescence property of quantum dots was utilized for sensitive detection of methyl para- thion at picogram level by using the strategy of competitive binding between free methyl parathion and CdTe quantum dots bioconjugate methyl parathion-immobilized anti-MP IgY antibodies and was observed in a flow injection sys- tem. This fluoroimmunoassay technique gives a sensitiv- ity of 0.1 ng mL−1 concentration within the time range of 10–15 min (Chouhan et al. 2010). In agricultural practices, deltamethrin (DM) is used for the control of a wide range of pest but has consequences such as high toxicity, long persis- tence, hard to degrade, and severe health issues. Thus, the tool for rapid and sensitive detection of deltamethrin was developed utilizing highly fluorescent silica nanospheres embedded cadmium tellurium quantum dots with a limit of detection of 0.16 µg mL−1(Ge et al. 2011).

In addition to several applications of metal nanoparticle- based nanosensors and nanobiosensors, the graphene oxide and functionalized carbon nanotubes control the efficient immobilization of entities on the surface which opens the door for construction of enzyme-based biosensors. With the advantage of guiding the protein orientation by reducing randomly bounded proteins to improve the sensitivity, the close confinement leads to efficient electron transfer between enzyme and electrode and simplifying the immobilization steps, thus improving the reproducibility and operability. Amino-functionalized carbon nanotubes control the effec- tive immobilization of AChE onto the surface of the glassy carbon electrode and use for development of a very deli- cate organophosphorus pesticide biosensor electrode. These electrodes have been successfully employed for detecting paraoxon and other pesticides from vegetable samples with a limit of detection of 0.08 nM (Yu et al. 2015).

The compatibility of carbon nanotubes and gold nano- particles provides a reference for the simultaneous use of the nanostructure in the construction of both nanosensors and nanobiosensors. The gold nanoparticles functionalized with electropolymerizable thioaniline were electropolymer- ized on glass surfaces along with the alkaline earth metal ions Mg2+, Ca2+, Sr2+, or Ba2+, to yield the respective ion- imprinted bis-aniline-bridged gold nanoparticle compos- ites. After removal of the ion from the composite, specific imprinted ion recognition sites were generated. Selective binding of the individual ions to the imprinted sites leads to the development of highly sensitive sensing method that can detect the ions even in femtomolar concentration (Ben- Amram et al. 2012).

Concanavalin A is a plant-derived lectin, specifically binding with the plasma membrane receptors containing mannose and glucose residues, and affecting the signaling to promote proliferation of the cells.  For senstive detection of

concanavalin A, first graphene oxide deposited on the gold sensor film followed by assembly of phenoxy-derivatized dextran over the graphene oxide-modified gold sensor chip surface via π–π interactions. The prepared graphene oxide/ phenoxy-derivatized dextran senses interface and specifi- cally captured concanavalin A which could further react with phenoxy-derivatized dextran–gold nanoparticle through the specific interaction between concanavalin A and phenoxy- derivatized dextran, forming a sandwich configuration and detected by surface plasmon resonance signal with the lesser concentration of 0.39  μg  mL−1. This method provides a designed surface plasmon sensor having high sensitivity, good selectivity, and reproducibility for concanavalin A detection (Huang et al. 2013).

With the progress in construction of carbon nanotube- based nanosensors, here self-assembled monolayers of single-walled carbon nanotubes fabricated by thiol-labeled oligonucleotide on gold nanoparticle were utilized to prepare nanometer size polyaniline matrix for acetylcholinesterase enzyme immobilization. The electrochemical biosensor con- structed detects pesticides methyl parathion and chlorpyrifos up to limit of detection 1 × 10−12 M (Viswanathan et al. 2009). In another strategy, multiwall carbon nanotubes, chi- tosan, and AChE liposomes bioreactor layers were combined to construct a multilayer film on glass electrode and used to detect organophosphate such as dichlorvos up to detection limit of 0.68 ± 0.076 µg L−1 by electrochemical measure- ment (Yan et al. 2013).

Acetamiprid is neonicotinoid-based pesticide acting as a neurotoxin by causing agonistic effects against nicotinic acetylcholine receptors (Shi et al. 2013). Aptamer-controlled reversible inhibition of gold nanozyme (nanoparticles enzyme mimicking) activity for acetamiprid sensing has been utilized for the sensing. The peroxidase-like activity of bare gold nanoparticle to oxidize colorless TMB into a purplish blue product and specificity of the acetamiprid-spe- cific S-18 aptamer to detect neurotoxic pesticide in a highly rapid, accurate and sensitive manner allowed the detection of 0.1 ppm acetamiprid within the assay time of 10 min (Weer- athunge et al. 2014). Moreover, in alternative strategy gold nanoparticles decorated multiwall carbon nanotube-reduced graphene oxide nanoribbon composites developed as ultra- sensitive label-free electrochemical impedimetric aptasensor for acetamiprid detection even with an extremely low detec- tion limit of 1.7 × 10–14 mol dm−3 (Jampilek and Kral’ova 2015).

Chitosan–Prussian blue–multiwall carbon nanotubes–hol- low gold nanospheres film was deposited on the gold elec- trode surface utilizing electrodeposition method. The ace- tylcholinesterase and Nafion were modified on the film to prepare an AChE biosensor. Prussian blue oxidizes thio- choline, which is the product of the hydrolysis of acetylthi- ocholine catalyzed by AChE (Sun and Wang 2010). This

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biosensor can sense pesticides such as malathion, chlorpyri- fos, monocrotophos, and carbofuran (Zhai et al. 2013).

Industrial wastes are the credible source of bromine ion which contaminates the environmental water and at elevated concentration pose the adverse side effect. In turn, a mul- tiwall carbon nanotube–chitosan modified glassy carbon electrode was utilized for sensitive cathodic stripping vol- tammetric measurements of bromide (Br−) with the limit of detection of 9.6 × 10−8 µg mL−1 (Zeng et al. 2005).

Carbofuran (2,3-dihydro-2,2-dimethylbenzofuran-7-yl methylcarbamate), a broad-spectrum insecticide widely used in agriculture, was quantitated by an amperometric immunosensor. The monoclonal antibody specific to carbo- furan was covalently immobilized on the gold nanoparticles using glutathione. Multiwall carbon nanotubes and graphene sheet–polyethyleneimine polymer–gold nanocomposites modified onto the surface of a glass carbon electrode via self-assembly. The modified graphene sheet–polyethyl- eneimine polymer–gold electrode was coated with gold nanoparticles–antibody conjugate which has been detected by the simultaneous amperometric immunosensing method with the limit of detection of 0.03 ng mL−1. The correlated electrochemical and immunological strategy gives a high specificity, good reproducibility, acceptable stability, and regeneration capability (Zhu et al. 2013).

Nanosensors for intelligent food packaging

The utilization of nanotechnology in food packaging is one of the promising applications, where nanoparticle and polymeric nanomaterial are being used to prevent the spoil- age by ceasing the gas, moisture loss. Much innovation has been made to incorporate the nanosensors and nanobiosen- sors at the time of packaging that persists with the food stuff and detect the food condition, freshness, and aroma. The nanosensors are being integrated into the packaging’s to sense the storage condition by estimating the physical parameter such as temperature, humidity, pH, oxygen con- tent, pathogens, toxins, and freshness by estimating the fer- mented by-product in the preserved food.

OxyDot® is the commercialized nanosensor being used to quantitate the dissolved oxygen into the packaged food and sealed drink product. The principle behind oxygen measurement technique is fluorescence intensity and life- time quenching of the metallic–organic fluorescent dye immobilized on the gas permeable hydrophobic polymer dot. The excitation wavelength of the dye falls into blue light reason and emits in the red spectrum. The presence of oxygen in the proximity and high collision dynamics in it withdraws the excited electron of the dye molecule and

in turn quenches the fluorescence and fluorescence lifetime of the dye. The OxyDot proves to be a reliable, sensitive up to 5% of reading, nondestructive, and rapid (less than 0.1 s) oxygen sensing technique that can measure the oxy- gen concentration in real time.

The insignia CO2 detection pallet intelligent labels and SMART DOTS are designed utilizing a cost-effective pig- ment system that exhibits a quick response to the CO2 con- centration and temperature change. Similarly, one another patented product named RipeSense® labels is intelligent ripeness indicator developed to detect the volatile com- pound released by the ripened food. The detection output is simply based on the color change of the label from red to orange and finally into the yellow.

The time–temperature indication is needed in process- ing and storage of the temperature sensitivity food stuff or material. The Timestrip Plus®, Timestrip Complete and 3 M MonitorMark are the patented time–temperature indi- cator. The construction of the indicator strip is done that it consists a combination of sensor and response element. The sensor system senses the temperature breach, and pigment system gives a differential color generation that strongly depends on the change of the temperature in refer- ence to calibrated temperature point. The Timestrip Plus is manufactured specific to different temperature range start- ing from − 20 °C to 86ºF from the time breach range of 12 to 48 h, whereas the Timestrip Complete equipped with the intelligent recognition and generated response as white to red on deciding 2 °C breach otherwise white to blue on ascending 8 °C breach. The 3 M MonitorMark gives the similar response in the temperature range of 15–31 °C.

Fresh Check is another time temperature indicator manufactured by TEMPTIMES, generally be used for the health and food stuff to be stored for a long time. Addi- tionally, the smart time–temperature Indicator developed by Vitsab International, CoolVu Food and Innolabel func- tions on a similar principle and used as an indicator in the refrigerated fruits, vegetables, and food product. Recently, the thermochromic inks-based colored thermometer labels and strips have been developed by Chromatic Technolo- gies, Inc and Matsui International, the USA, for its diverse application in retail food safety and storage.

Toxin Guard is an antibody-based biosensing approach developed by Toxin Alert, Canada, for detection of patho- genic bacteria such as Salmonella sp., Campylobacter sp., E. coli, and Listeria sp. The strategy utilized is the use for pathogen-specific antibodies in the plastic wrap used for the food packaging, and the accumulation of the labeled detector antibodies after interaction with the contaminant in the particular area gives a visible colored indication of the presence of toxin and pathogens.

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Intellectual property rights and recent patents

Intellectual property rights are the legal rights obtained on creativity or inventions, which allow the holder to prevent unauthorized open use of their inventions. Generally, IPRs are broadly demarcated into two sections; the first comprises the property, patents, trademarks, and industrial design, whereas second domain deals with the copyright of artis- tic creatures, literary works, performances, and broadcasts (Bastani and Fernandez 2002). The patent system gives an exclusive flexibility to defense when any challenge of the ownership has been raised with clear documentary evidence of terms of boundary and area of protection (Hwang et al. 2016). Trade-Related Aspects of Intellectual Property Rights Agreement abbreviated as TRIPs within the World Trade Organization has certain framework criteria and eligibility of issuing the patent rights mentioned in the Article 27 of “Patentable Subjects Matter” (Kochhar 2008). The United State Patent and Trademark Office (USPTO), European Patent Office (EPO), and Japan Patent Office (JPO) are the three major organizations which provide the patent right in area of nanotechnology. The EPO made the classification of the nanotechnological inventions under Y01 N, which is further subcategorized in several classes such as Y01N2,

nanobiotechnology or nanomedicine; Y01N4, nanotechnol- ogy for information processing, storage, and transmission; Y01N8, nanotechnology for material and surface science; Y01N10, nanotechnology for optics; and Y01N12, nanomag- netics (Ranjan et al. 2016). Recently, several patent rights have been issued in area of nanosensors which have direct applicability in the detection. The strip-based nanosensors have been developed by utilizing the nanoplatform assembly of two different colorimetric nanoparticles linked with the protease consensus sequence or ester linkage. The protease enzyme present in the milk product cleaves the amino acid sequence of consensus, and because of the enzymatic activ- ity and plurality of the nanoparticles, a visual color change is generated. The patented nanosensor approaches have impli- cations in the detection of enzymatic activity in dairy prod- uct for further safety (Troyer et al. 2016, WO2016018798 (A1)). In another approach, the molecular imprinted conduc- tive polymer and gold nanoparticle nanojunction have been used for the construction of molecular imprinted nanosensor device and could be used for the detection of desirable ana- lytes (Li et al. 2013, US2013092547 (A1)). Many instances of the recent patents rights are mentioned in Table 3; with the respective analyte, nanostructure has been utilized and the mode of detection. The innovation in the area of sen- sors and its commercialization still needed thrust that could

Table 3 Recent patents globally accepted  under nanosensors and nanobiosensors

The table represents the detection application, nanostructure used in the construction of nanosensor, mode of detection, and the patent detail with the year of approval (left to right)

Detection Nanostructure used Mode of detection Patent ID/year

Chemical analyte Graphene functionalized with aptamer Electrochemical WO2016112079 (A1) (2016)

Chemical or biological agent Silver and gold nanoparticles Surface plasmon resonance US2016161407 (A1) (2016)

Water quality Single-walled carbon nanotubes Microfluidics US2016129455 (A1) (2016)

Ammonia Semiconductor nanoelectronics Electrical US2016123947 (A1) (2016)

Enzyme activity in dairy product Nanoparticle assembly Colorimetric WO2016018798 (A1) (2016)

Nucleic acid Nanowires Electrical US2016033498 (A1) (2016)

Pathogenic bacteria Hybridizing magnetic relaxation nanosensors Electrical US2014220565 (A1) (2016)

Chemical analyte Photoluminiscent carbon nanotubes Optical US2014080122 (A1) (2014)

Chemical analyte Molecular imprinted conducting polymer nanojunctions Electrochemical US2013092547 (A1) (2013)

Pathogens Quantum dots Optical US2011177585 (A1) (2011)

pH in food sample Functionalized nanoparticles Electrochemical US2010330686 (A1) (2010)

Toxins and contaminants Luminescent protein–Quantum dots Optical WO2006083269 (A2) (2006)

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be possible with the flexibility in the academia–industrial participation, amendments in the rule patents right and ulti- mately making the smooth patent application process.

Conclusion

Research activity and innovation in the areas of nanosensors and nanobiosensors have extraordinary growth in the last one decade. This chapter made an effort to provide the cur- rent trend and innovation in nanosensors and nanobiosensors construction or designing along with their potential applica- tions in the area of food and agriculture sector. The kind of nanomaterials such as gold nanoparticle, silver nanoparticle, magnetic iron oxide nanoparticle, quantum dots, graphene oxide, single-walled and multiwalled carbon nanotubes has been used preferably because of unique chemical, optical, thermal, and mechanical properties. Incorporation of these nanoparticles via covalent/non-covalent linkage and fabrica- tion in the sensing component has enhanced the sensitivity and specificity of the sensors. The construction and work- ing principles of recent nanosensors such as nanobarcode technology, electronic nose and electronic tongue, wireless nanosensors, rapid detection technology, optical nanosen- sors have been extensively discussed. The application of the nanosensors and nanobiosensors in the area of food technol- ogy from detection of food preservative contaminants and food-borne microbial load to agriculture sector for the pres- ence of the pesticides, herbicides, heavy metal ions, and fer- tilizer residues have been extensively reviewed. In reference to increasing applications of the nanomaterial-based sensor in the area of agriculture and food sector; many advance- ments are anticipated.

Acknowledgement The author gratefully acknowledges the financial support from Council of Scientific and Industrial Research (CSIR), New Delhi, and Science and Engineering Research Board (SERB) grant: ECR/2016/000633/LS.

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