Engineering in Agriculture, Environment and Food xxx (2016) 1e12

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Engineering in Agriculture, Environment and Food

journal homepage: http://www.sciencedirect.com/eaef

State of ion mobility spectrometry and applications in agriculture: A

review
Gopi Krishna Kafle a, Lav R. Khot a, b, *, Sindhuja Sankaran a, Haitham Y. Bahlol b, c,
Jessica A. Tufariello d, Herbert H. Hill Jr. d
a
Biological Systems Engineering Department, Washington State University, Pullman, WA 99164, USA
b
Center for Precision and Automated Agricultural Systems, Irrigated Agriculture Research & Extension Center, Washington State University, Prosser, WA
99350, USA
c
Foundation of Technical Education, Baghdad, Iraq
d
Department of Chemistry, Washington State University, Pullman, WA 99164, USA

a r t i c l e i n f o a b s t r a c t

Article history: Ion mobility spectrometry (IMS) has been employed successfully to detect chemicals such as explosives,
Received 3 April 2015 illicit drugs, chemical warfare agents, pharmaceutical chemicals, and environmental pollutants. However,
Received in revised form applications of IMS in pre- and post-harvest agriculture production management has not been explored
1 April 2016
adequately. Characteristics such as high sensitivity, selectivity, analytical flexibility, field portability, and
Accepted 14 May 2016
real-time monitoring abilities offer great potential of IMS applications in agriculture. In this paper,
Available online xxx
reviewed are the different types of IMS, their working principles, and agricultural applications. Some of
the agricultural applications include; detection of contaminants affecting soil and plants, assessing plant
Keywords:
Volatile organic compounds
stress, and monitoring postharvest agricultural produce quality and safety.
Agriculture Published by Elsevier B.V. on behalf of Asian Agricultural and Biological Engineering Association.
Biotic and abiotic plant stress
Post-harvest loss management

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2. Advances in ion mobility spectrometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3. IMS applications in agriculture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.1. Assessing soil contamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.2. Toxic chemical detection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.3. Plant stress monitoring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.4. Evaluating produce quality . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.5. Other pertinent applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
4. Summary and future research thruts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00

Abbreviations: AIMS, Aspiration ion mobility spectrometry; CD, Corona

discharge; DMS, Differential mobility spectrometry; ESI, Electrospray ionization;
FAIMS, Field asymmetric ion mobility spectrometry; GC, Gas chromatography; IMS,
Ion mobility spectrometry; K0, Ion mobility at standard temperature (273 K) and
pressure (1 atm.)(cm2/(V
s)); LC, Liquid chromatography; LC/MS, Liquid
chromatography-mass spectrometry; MCC, Multiple capillary column; MESI,
Membrane extraction with a sorbent interface; MS, Mass spectrometry; NMR,
Nuclear magnetic resonance; NTD, Needle trap devices; SPME, Solid phase micro-
extraction; SS-IMS, Subsurface-ion mobility spectrometry; TW-IMS, Travel wave-
ion mobility spectrometry; UV, Ultraviolet; VOC, Volatile organic compound.
* Corresponding author. Biological Systems Engineering Department, Washing-
ton State University, Pullman, WA 99164, USA.
E-mail address: lav.khot@wsu.edu (L.R. Khot).

http://dx.doi.org/10.1016/j.eaef.2016.05.004
1881-8366/Published by Elsevier B.V. on behalf of Asian Agricultural and Biological Engineering Association.

Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
2 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12

References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00

1. Introduction have been developed into field portable systems for warfare
chemicals and illegal narcotics detection (Cumeras et al., 2015b).
Pre- and post-harvest crop management is critically important The other common IMS applications are towards 1) detection of
in agriculture worldwide. Proper agricultural produce management drugs and explosives in civil airports, 2) detection of chemical
through integrated sensing based decision-making will not only weapons in combat areas, and 3) investigation of ion-molecule
result in preventing economic losses to the producers; but also will reaction, ion structure, and conformation of biomolecules such as
address aspects of global food security. For example, early detection peptides and proteins and separation of isomers (Arce and
of plant diseases and disorders (before the onset of disease symp- Valcarcel, 2013). Review of scientific publications indicate that
toms) could be vital for implementing proper pest management about 36% of IMS applications are in explosives and chemical
and disease control strategies. Similarly, rapid sensing for post- warfare detection, 21% in pharmaceutical and drugs, 14% in clinical
harvest food quality monitoring throughout packaging and market and biological studies, 9% in environmental studies, 8% in quality
supply-chain can reduce the agricultural produce losses and might control, 5% in food, 5% in forensic, and 2% in industry and other
improve consumer perception. Therefore, academia and industry fields (Arce and Valcarcel, 2013). The portability, high sensitivity,
have put enormous thrust towards development and evaluation of accuracy, ease of optimization, and a fast response time (ms) at
non-contact rapid sensing modules for pre- and post-harvest pro- room temperature and atmospheric pressure makes IMS a pro-
duce management. Prior and ongoing research suggests that spective sensing system for detecting volatiles in diverse environ-
several sensing approaches and techniques have been explored to ment (Harden and Shoff, 1997; Pollard et al., 2011). Moreover, IMS
address this aspect. One such approach is volatile organic com- technology offers chemical profile data with higher qualitative and
pounds (VOCs) or biomarker-based sensing. quantitative accuracy during measurements, although it is more
Naturally, plants and agricultural produce release key volatiles expensive than photoionization detectors and e-noses (Arce et al.,
that can be associated with their morphological and physiological 2008; Mayer and Borsdorf, 2014). IMS based non-contact sensing
status, which can be affected by abiotic/biotic stress factors and technologies has not been applied widely in agriculture. Thus, the
other disorders. These VOCs or the VOC profile can be an indicator major focus of this review will be towards agricultural applications
of plant or produce condition. VOC-based sensor technologies that include: soil contamination assessment, toxic chemicals
facilitate non-invasive, real-time detection of biological volatiles detection, plant stress monitoring, produce quality and safety, and
can be utilized to prevent the crop losses, improve agricultural other pertinent applications such as food and beverage, and wood
management practices, and ultimately provide economic benefits quality (DeBono et al., 2001; Vautz et al., 2004b; Vautz et al., 2006;
(Sankaran et al., 2010). Dudareva et al. (2006) reviewed a range of Borsdorf et al., 2009; Zhang et al., 2011; Owlstone, 2013; Aksenov
volatiles released by the plants under stress such as terpenoids, et al., 2014; Rutolo et al., 2014).
phenylpropanoids and benzenoids, volatile fatty acids (trans-2-
hexenal, cis-3-hexenol and methyl jasmonate), and amino acid 2. Advances in ion mobility spectrometry
volatiles (such as aldehydes, alcohols, esters, acids, and nitrogen-
and sulfur-containing volatiles derived from amino acids), which The working principle of IMS is illustrated in Fig. 1a. An IMS
can be used for such applications (Sankaran et al., 2010). consists of four main components: 1) sample introduction system,
Different techniques have been used to evaluate volatiles qual- 2) molecule ionization source, 3) drift tube for separation and se-
itatively and quantitatively. Most common techniques of biogenic lection of ions, and 4) ion detector (Ma
rquez-Sillero et al., 2011).
VOCs determination are based on purge-and-trap or headspace The drift tube is considered the heart of an IMS where ions are
sampling methods, such as solid-phase micro extraction (SPME), created utilizing the ionization source under the electric field and
followed by gas chromatography-mass spectrometry (GC-MS) allowed to migrate (Hill et al., 1990). Normally, Faraday plates are
analysis (Fellman et al., 1993). However, sample preparation for GC- used as the detector and to measure ion current in IMS instruments
MS analysis can be time consuming, expensive, and requiring (Fig. 1a).
specific skills for proper operation. Thus, such techniques of VOCs Once the sample is introduced through a carrier gas into the
monitoring may not be applicable for rapid volatile monitoring in ionization chamber, it is ionized to form different ions (positive or
agriculture (Laothawornkitkul et al., 2008; Ciesa et al., 2013). negative ions) depending on the ionization source. These ions are
Similarly, technologies such as proton transfer reaction-mass transferred to the separation chamber (drift region) via an elec-
spectrometer (PTR-MS), nuclear magnetic resonance (NMR), and tronic grid. Drift region/tube contains an electric field and drift gas
liquid chromatography-mass spectrometry (LC/MS) are capable of that separates the ions according to mobility (Ma
rquez-Sillero et al.,
providing more comprehensive chemical information (the semi- 2011). Smaller size ions moves faster and reach the detector earlier
volatiles and higher molecular weight plant metabolites) but are than larger ions. A collector (Faraday plate) detects the arrived ions
limited to laboratory settings (Alexander et al., 2013). In compari- and generates a current. The generated current is amplified for
son to MS and other methods discussed above, electronic nose (e- producing a mobility spectrum. The ion mobility (K0) is defined as
nose) is faster, less expensive, and can be used in field conditions the ratio of the ion velocity to the magnitude of electric field (Hill
without the requirement of sample preparation. Yet, some of the et al., 1990) and is dependent on characteristic properties of a
limitations include: 1) poor reproducibility, 2) lower resolution sample (i.e. size, charge and mass of the ion). At the detector, ions
signal drift, 3) difficulty in correlating e-nose responses with other collide and annihilate, and resulting ion current is recorded with
analytical sensor outputs, and 4) challenges in identifying and respective time stamp (Ma
rquez-Sillero et al., 2011). Thus, a plot of
quantifying specific compounds (Zhang and Li, 2010; Sankaran ion current against K0 forms an ion mobility spectrum, with cor-
et al., 2012; Alexander et al., 2013). responding ion mobility bands to each of the unique ionic species
Recently, handheld ion mobility spectrometry (IMS) modules (Fig. 1b). The spectrum is a fingerprint of the parent compounds.

Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12 3

Fig. 1. Schematic representation of the (a) ion mobility spectrometry working principle and (b) resulting ion mobility spectrum.

An IMS performance is defined by the selectivity and sensitivity,
and could be governed by operating electric field, type of buffer gas,
and pressure variation at drift tube (Purves and Guevremont, 1999).
The ionization source is one of the factors that govern the selec-
tivity of the IMS unit. Radioactive sources such as Nickel-63 (63Ni),
Americium-241 (241Am), Tritium (T or 3H), and non-radioactive
sources such as CD, photoionization, electrospray ionization (ESI)
and laser-based ionization are commonly used in commercial units.
Among these, 63Ni is most commonly used ionization source, fol-
lowed by corona discharge ionization (atmospheric pressure)
(Eiceman et al., 2013). Roscioli (2012) reported that the CD has
several advantages over 63Ni sources including low cost for con-
struction materials, ease of operation, and the capability of gener-
ating greater ion currents. UV light or electric discharges has also
been used to ionize the sample in an IMS unit (Baumbach, 2006).
More details about different ionization sources along with their
positive and negative features are described in Guharay et al.
(2008).
The type of operation polarity (positive or negative) can also
affect selectivity of IMS response. Electropositive compounds (such
as drugs and amines) show good responses as positive ions and
electronegative compounds (such as explosives) are detected well
as negative ions (Hill and Simpson, 1997). For improved selectivity,
doping agents can be added to the drift gas for controlled ioniza-
tion. For example, Kim et al. (1978) used low levels of ammonia
doping for the strong gas-phase bases (e.g. amines and drugs) to
improve IMS response. Similarly, Lawrence and Neudorfl (1988)
experimented with the addition of dichloromethane under nega-
tive ionization mode to enhance the electronegative explosives
responses. Generally, ions are characterized according to their
mobility in a drift gas under electric field influence. Thus, changing
the drift gas identity (mass and polarizability) can influence the
IMS separation capabilities (St. Louis et al., 1990). Pre-separation
techniques can be additional option for increasing IMS selectivity
(Vautz et al., 2004a).
For complex mixtures, it is hard to identify each analyte due to
confounding mobility for several analytes. In such conditions, hy-
phenated methods are useful (Borsdorf and Eiceman, 2006;
Cumeras et al., 2015a) for versatile applications. A common hy-
phenated technique includes coupling IMS with MS system known
as ion mobility-mass spectrometry (IM-MS) in which IMS works as
pre-filter by confirming ion identities for MS systems. Major benefit
of IM-MS is that an IMS can separate isomers of the same chemical
compounds and MS identifies those compounds (Kanu et al., 2008).
Second approach is to pre-separate sample prior to the IMS sensing.
This strategy is used for both gases and liquids (Cumeras et al.,
2015b). A GC and multi capillary columns (MCC) are commonly
used for pre-separation in the gas-phase. In GC-IMS or MCC-IMS
systems, GC or MCC pre-separates the sample before entering the
IMS (Kanu et al., 2008; Cumeras et al., 2015a). Pre-separation
techniques such as GC and MCC are used to analyze complex
mixtures including several analytes with similar mobilities because
they allow additional options for separation of analytes based on
retention times (Xie et al., 2002; Baumbach et al., 2003). Addi-
tionally with pre-separation systems, it is possible to detect the
relevant analytes even at 100% relative humidity without any
negative effects (Vautz et al., 2004a). Similar to liquid chromatog-
raphy (LC) use prior to MS detection (Schwanhausser et al., 2011),

Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
4 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12

coupling of an IMS drift cell between the LC separation and MS has
multiple advantages for analyzing complex mixtures (Cumeras
et al., 2015b).
To summarize the developments in IMS technology, to date six
most common IMS types exist in the market. Those include drift
time IMS (DT-IMS), traveling-wave IMS (TW-IMS), high-field
asymmetric waveform IMS (FAIMS), trapped IMS (TIMS), aspira-
tion IMS (AIMS), and differential mobility analyzers (DMA)
(Cumeras et al., 2015a). Special features of these IMS are illustrated
in Fig. 2. Selected commercial IMS types suitable for agricultural
applications along with distinguishing features are summarized in
Table 1. More specific details on each of these types and pertinent
operating conditions can be found at Kanu et al. (2008), Owlstone
(2014), and Cumeras et al. (2015a).
3. IMS applications in agriculture
3.1. Assessing soil contamination
The recent site activities, past land use, and short distances from
pollution sources affects the properties of the soil; in addition to
fertilizers, pesticides, or other amendments for desired applica-
tions. Similarly, chemical spills or leaks can also contaminate the
soil strata. For example the disposal of solvent waste generated
from textile industries and dry cleaner to the soil causes leaching of
trichloroethylene (TCE) and tetrachloroethylene (PCE) into the soil,
which can contaminate both soil and ground water (Kanu et al.,
2007; Tabernacka et al., 2014). Use of toxic chemical warfare
agents (CWAs) such as organophosphorus compounds can be
another source of contamination in the soil (Rearden and
Harrington, 2005), that can result in serious illnesses and some-
times even death (Moretto, 1998). Similarly, presence of heavy
metals such as Zn, Cr, Cu, Cd, Pb, Co and Ni can contaminate (Ene
et al., 2010), and cause an increase of ethylene production in the
soil (Goren and Siegel, 1976; Burd et al., 2000). These factors can in-
turn inhibit the development of root and shoot, reduce CO2 fixation,
and translocation of sugar (Prasad and Strzalka, 2002). One of the
potential applications of IMS can be in evaluating the soil quality,
which can include agricultural regions. Table 2 summarizes some
examples where IMS has been used to detect few soil contaminants
discussed above.
Kanu et al. (2007) reported field use of IMS for the detection and
separation of TCE, PCE, and nine other environmental soil-gas
contaminants (Table 2). A subsurface IMS (SS-IMS) was used un-
der positive ion mode for detecting TCE and PCE. Study concluded
that the SS-IMS was effective for detection as well as separation of
environmental soil-gas contaminants. Study also reported that IMS
technology might lead to a simple and practical approach
compared to other technologies such as GC-MS and HPLC for long-
term monitoring of the soil contaminants. In another study,
Kuperman et al. (2003) coupled solid phase micro-extraction
(SPME) with IMS to detect precursor and degradation products of
CWAs such as diethyl methyl phosphonate (DEMP), diisopropyl
methyl phosphonate (DIMP), and dimethyl methylphosphonate
(DMMP) as soil contaminants. The use of SPME improved the
reproducibility and offered rapid screening of soil contaminants (as
low as 10 mg/g). Overall, studies on soil contaminant detection using
IMS are sparse but the potential of this technology is prudent.
3.2. Toxic chemical detection
Various toxic chemicals (pesticides, herbicides) are used for
controlling weeds, insects, and diseases in plants all over the world.
Although agricultural productions can be increased tremendously
using these chemical applications, there are possibilities for traces
of these chemicals to be present in the plants and their produce
that can cause health risks to workers and consumers. The IMS
technology has been used to evaluate some of these chemical res-
idues. Few examples are as summarized in Table 2.
Tuovinen et al. (2000) reported the use of AIMS for identifying
different pesticides (organo-phosphorus compounds as diazinon,
dimethoate, and parathion and carbamate compounds as aldicarb)
from liquid matrices. For such detection, the study recommended
positive channels to measure pesticides at lower concentrations. It

DT-IMS TW-IMS FAIMS/DMS

Sensitivity: low
Selectivity: -
Resolving power: high
Operating pressures: ambient
Mode: +ve or -ve ion
Salient feature: can be integrated
with commercial MS systems
Sensitivity: high Sensitivity: high (> TW-IMS)
Selectivity: medium Selectivity: high
Resolving power: high Resolving power: low
Operating pressures: 0.025-3 mbar Operating pressures: ambient
Mode: +ve and -ve ion Mode: +ve and -ve ion
Salient feature: easy integration Salient feature: handheld, field
into commercial MS systems portable systems

T-IMS
Sensitivity: low (> DT-IMS)
Selectivity: -
Resolving power: high
Operating pressures: 2.6-3.4 mbar
Mode: +ve and -ve ion
Salient feature: do not require
high voltage to achive high
resolving power and can be well
integrated with MS system
A-IMS
Sensitivity: medium (>DT-IMS)
Selectivity: -
Resolving power: low (<DT-IMS)
Operating pressures: ambient
Mode: +ve and -ve ion
Salient feature: handheld, rapid
and low energy consumption
DMA
Sensitivity: medium to high
Selectivity: -
Resolving power: medium to high
Operating pressures: 80-1000
mbar
Mode: +ve and -ve ion
Salient feature: can be very useful
in classifying and generating
mono disperse particles

Fig. 2. Typical IMS types with key features. DT-IMS: Drift tube IMS; TW-IMS: Traveling wave IMS; FAIMS/DMS: High field asymmetric waveform ion mobility spectrometer/dif-
ferential mobility spectrometry; TIMS: Trapped IMS; AIMS: Aspiration IMS; DMA: Differential mobility analyzer; MS: Mass spectrometry (information acquired from Intra and
Tippayawong, 2008; Kanu et al., 2008; Owlstone, 2014; Cumeras et al., 2015a).

Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
 Table 1
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in

Details of selected commercial IMS units that can be appropriate for agricultural applications.a

Company name Owlstone, Nanotech Ltd., Schumann-Analytics, GAS, Dortmund, German RAMEM S.A, Modrid, EXCELLIMS corporation, Environics-IUT GmbH,
Cambridge, U.K. Einbeck, German Spain MA, U.S.A. Berlin/Adkershof, German
Product Lonestar GC-FAIMS MCC-IMS FlavourSpec® IONER High Resolution GA2100 HPIMS IMS MINI-200
IMS
Working principle FAIMS Pre-separation via gas GC-IMS GC-IMS FAIMS/DMS Combining electrospray IMS
chromatographic column, Ion mobility spectrometry Ion mobility spectrometry ionization (ESI) with high
detection with a high with chromatographic with chromatographic resolution IMS technology
FAIMS detector pre-separation pre-separation
Portable Yes No e No No No Yes
63 63
Ionization method and Ni or ultra violet (UV) Ni or UV Radioactive ß-radiation, ß-radiation source (3H) UV light (photo ESI with changeable ion Tritium (3H)
source Tritium (3H) ionization), 10.6 eV source
lampand other ionizations
options (electrospray,
corona, radioactive (63Ni

G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12
or 241Am))
Detection limit ppt-ppb Low ppb range Low ppb or mg/L range Low ppb range Low ppb range Low ppb range Low ppb range
Analyte range Industrial gases and VOCs Volatile, semivolatile and VOCs in complex matrices VOCs in food and Aerosols and VOCs A wide range of Toxic gases and chemical
(Application) nonvolatile organic (e.g. ketones, aldehydes, beverages compounds including warfare agents
compounds in complex alcohols, amines and isomers and those that are
matrices phosphor organics as well chromatographically
as halogenated sensitive or lack a UV
compounds) chromophore
Application domain Food freshness and odor, Water contaminants (e.g. Beverage industry Control of storage Environment, security, Chemicals, Agriculture (H2S, NH3,
food and beverage taints, pesticides), trace (process and quality conditions, food food inspection, diagnosis pharmaceuticals, food and pesticides), food
diseases in stored food impurities in polymer and control in wine and beer freshness, control of beverages industry(quality control,
(e.g. potato), fermentation solid samples, toxicology production), food production process, (contamination, flavors), medicine, water
and bioreactor off-gas analyses, indoor air freshness (e.g. fish process optimization, pesticides, flavors, pollution control, liquid
analysis, pharmaceutical quality, flavor analyses of spoilage), sensitive VOCs flavor evaluation and fragrances) waste, security, building
solvent drying, etc. food products, detection detection (e.g. acetone in flavor stability, test of raw protection, storage of
of toxic industrial human breath) materials, product hazardous materials and
compounds (e.g. BTEX), authentication waste, etc.
medical, detection of
wood preservatives
Sample phase Gas, liquid, solid Gas, liquid, solid Gas Gas e Gas, liquid, solid Gas
Sample input Ambient, headspace, Heated injector, direct Heated electrical 6-port- Automatic GC headspace Direct or with membrane Gas and solid by thermal Direct gas sampling in
process line injection via a syringe or valve (stainless steel), gas injector and VOCs in the desorber, and liquid by headspace
by solid phase micro tight loop (1-10 mL) headspace of solid and flow cell or direct spray
extraction (SPME) or six liquid samples
port valve
Detection mode Positive and negative Positive and negative Positive or negative, Positive and negative, Positive and negative Positive and negative Positive and negative,
switchable switchable switchable automatically
during detection
Carrier gas Air N2 or air for FAIMS and N2 N2 N2 e e No carrier gas needed
or air for GC
Startup time (min) 5 e 5 e e e 15
Analysis time <1s e Few seconds 3e7 min 1e5 min Matter of seconds Few seconds
Weight (kg) 7.8 e 15.5 25.5 25.0 e 6.5 (including battery)
Reference Rutolo et al., 2014 Schumann et al., 2012 Ruzsanyi et al., 2012 GAS, 2014 Santos et al., 2009 Midey et al., 2013 Eiceman et al., 2013

IMS: Ion mobility spectrometry; FAIMS: Field asymmetric ion mobility spectrometry; DMS: Differential mobility spectrometry; GC-MS: Gas chromatography-mass spectrometry; MCC: Multiple capillary column; VOCs: Volatile
organic compounds.
e: Information not available.
a
List is not all-inclusive and authors do not intend to promote any particular unit rather point to such units of which variants may be available in the market.

5
6 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12

Table 2
Typical IMS applications in sensing of toxic chemical in soil and plants.

Sample Target analytes Detection limit IMS type Ionization source Study purpose Reference

Soil contaminants
Soil spiked Diisopropyl methylphosphonate mg/g PCAM® type 482-301N e Detect chemical warfare Rearden &
(DIMP), diethyl (Graseby Ionics, precursor and degradation Harrington, 2005
methylphosphonate (DEMP), and Watford, Herts., U.K.). products in soil
dimethyl methylphosphonate
(DMMP)
63
Soil-gas Trichloroethylene (TCE), ppb SS-IMS Ni Detect environmental soil- Kanu et al., 2007
contaminants tetrachloroethylene (PCE), gas contaminants
methylene chloride (DCM), 1,2-
dichloroethane (DCE), 1,2,4-
trichlorobenzene (1,2,4-TCB),
methyl tert-butyl ether (MTBE),
methyl iso-butyl ketone (MIBK),
acetone, toluene, p-xylene and
ethylbenzene
Plant contaminants
Pesticides or Diazinon, aldicarb, dimethoate and ng or mg AIMS (MGD-1, AM241 Detect pesticides from a Tuovinen et al., 2000
insecticides parathion Environics Oy, liquid matrix
(organophosphate Kuopio, Finland)
and carbamate)
63
Cherry tomatoes Malathion and dichlorovos ng/L Portable IMS Ni Detect contaminants in Wang et al., 2011
cherry tomatoes
Potato and drinking Nitrite and nitrate mg/L ESI-IMS Corona discharge Detect nitrite and nitrate, Jafari et al., 2012
water simultaneously in water
and potato

IMS: Ion mobility spectrometry; PCAM: Portable Chemical Agent Monitor; SS-IMS: Subsurface IMS; AIMS: Aspiration IMS; ESI-IMS:Electrospray ionization IMS.

was reported that AIMS detection sensitivities for various analytes
(pesticides) decreased in the order of diazinon, aldicarb, dimeth-
oate, and parathion. Overall, the study showed the possibility for
the use of IMS in detecting some of the insecticide compounds in
liquid matrix. It was also claimed that method used in the study
could be adopted in flower growing greenhouses in order to
monitor pesticides compounds in air or foliage. In another study,
Wang et al. (2011) evaluated a handheld IMS for detecting chemical
contaminants (malathion and dichlorovos traces) on cherry to-
matoes. The experimental results showed that IMS offered a simple,
rapid, and acceptably reproducible approach with the relative
standard deviations of 8.4% and 7.2% for dichlorovos and malathion
detection, respectively.
The major sources of nitrite and nitrate in the environment are
from the fertilizers used in agriculture. The reaction between nitrite
and secondary amines present in the food products forms nitro-
soamines in human digestive systems, which is harmful to human
health (Jafari et al., 2012). Nitrate is more stable and less toxic
compared to nitrite but nitrate is easily biodegradable and con-
verted into nitrite by microorganisms (present in food products).
Thus, a quick and highly sensitive technology is desirable to
determine traces of nitrite and nitrate from aqueous samples
directly (Jafari et al., 2012). Jafari et al. (2012) evaluated ESI-IMS
(with negative polarity) for detection of nitrate and nitrite in the
potato and water samples. ESI is non-radioactive source that con-
verts liquid molecules of the sample into aerosols. This ionization
source is attractive because it enables direct identification of
compounds (organic and inorganic) in liquid samples (Jafari et al.,
2012). Such method was found to be simple and very effective for
analysis of nitrate and nitrite simultaneously in the samples. Thus,
above studies revealed potential of IMS in detecting toxic chemicals
in agriculture. Further studies may be required to determine the
suitable type of IMS (ion source, polarity) for specific chemical
detections.
3.3. Plant stress monitoring
Plants undergo stress, when they are exposed to less than ideal
growing conditions. Plants can experience abiotic (drought, heat,
nutrient deficiency) and biotic (diseases, pest) stress, which can
affect the plant semiochemical production. Plant health can be
diagnosed non-destructively by monitoring these volatiles (semi-
ochemicals) emitted at different growth stages and under different
stress conditions. According to Knudsen and Gershenzon (2006),
about 1700 plant volatiles have been discovered from 90 families of
plants to date. These plant volatiles are mainly represented by
phenylpropanoids/benzenoids, terpenoids, and derivatives of fatty
and amino acids (Dudareva et al., 2004). Application of IMS tech-
nology in monitoring plant stress under field conditions can play
crucial role in reducing production losses and warrant more studies
as technology becomes readily available beyond the laboratory
environment. Below is the review of some pertinent research in this
area.
Environmental factors and physiological conditions of non-
biological nature can result in abiotic stress. Some of the exam-
ples include, drought, heat, and chilling conditions, nutrient de-
ficiencies, excessive agrochemicals (herbicides, pesticides etc.),
high uptake of salts, and heavy metals (Goren and Siegel, 1976;
Burd et al., 2000; Govindasamy et al., 2008). Govindasamy et al.
(2008) explained that the volatile hormones have the capacity to
diseases and environmental pressure in plants. There is a potential
to detect such volatiles using IMS.
Similarly, phytopathogens (fungi, bacteria and viruses), insects,
nematodes, weeds and other organisms can cause changes in vol-
atile profile released by the plants that can be monitored using IMS
technology. The technique can also be applied to postharvest pro-
duce quality as discussed in the next section. For instance, sensing
of specific volatiles produced during fruit ripening could help
determine the agriculture produce quality (Costa et al., 2007).
Moalemiyan et al. (2007) detected fungal diseases such as stem-
end rot and anthracnose in mangoes by employing VOCs profiling.
Several studies have also reported that the interaction between
plant and pathogens can induce release of specific kinds of volatiles
(Spinelli et al., 2006; Turner and Magan, 2004). In the study con-
ducted by Vuorinen et al. (2007), VOC emission trends from silver
birch were utilized to determine whether the plants were healthy,

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 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12
destroyed by larvae (herbivore), or infected with pathogenic leaf
spot. Linalool and ethyl salicylate was released from the leaves
damaged by herbivore, especially after 72 h of feeding. It was also
observed that the twigs that were infected by pathogen released
higher amounts of (Z)-ocimene and (E)-ocimene compared to the
control twigs. An early disease detection system can aid in
decreasing such losses caused by plant diseases and can further
prevent the spread of diseases (Sankaran et al., 2010), which can be
achieved using IMS technology. Example studies on IMS application
in plant stress detection are summarized in Table 3.
Aksenov et al. (2014) investigated a new approach for VOC
monitoring for early greening or Huanglongbing disease detection
in citrus using gas chromatography differential mobility spec-
trometry (GC-DMS). The samples were collected from healthy and
infected (varying degree of symptoms) citrus trees in the orchard
and in controlled environment. Phenotypic and physiological
changes occurring in the plants system were also monitored. The
394 samples (out of 427) were utilized for chemometric multivar-
iate analysis. The classification results (healthy and infected trees)
were examined quantitatively using multiway partial least squares
(MPLS). Based on the top five most discriminating compounds
(VOCs), the citrus trees were categorized into healthy or infected
(asymptomatic, mild, and severe). For in-field trees, VOCs results
showed huge difference between infected and uninfected trees
regardless of polymerase chain reaction (PCR) status. VOCs based
detection method used in this study showed >90% accuracy in
detecting greening diseases in citrus. The study indicated that early
disease detection using GC-DMS could be a novel and powerful
technique to track crop infections and this approach can be applied
to other crops and pathogens.
Zhang et al. (2011) used FAIMS under controlled environment
conditions to detect different types of diseases (powdery mildew,
spider mites) in tomato plants by measuring the chemical volatiles
emitted by the plants during the disease progression. Data
collected from FAIMS was processed using principle component
analysis (PCA) and results showed clear patterns on all the exper-
imental plants representing the gradual development of the dis-
eases. In another study, Wu (2009) coupled sample preparation
analytical systems such as needle trap devices (NTD) and mem-
brane extraction with a sorbent interface (MESI) with portable IMS
to detect a-pinene emissions from plants (pinus species and
Table 3
Examples of some studies on IMS application in plant stress detection.
Sample Target analytes
Pinus species and a-pinene
peppermint
Tomato Chemical volatiles emitted by tomato plants
with different health conditions (powdery
mildew infected, spider mites infected, and
health control plant)
Citrus tree Top five most discriminating compounds
(VOCs) identified for different health conditions
(Healthy, HLB þ but asymptomatic, HLB þ with
mild symptoms) are:
Healthy (geranyl acetone, hexacosane,
pentadecane, linalool, (n-) tetradecanol)
Asymptomatic ((1-) tetradecene, linalool,
nonadecane, phenylacetaldehyde,
ethylhexanol)
Mild ((trans-2-tert-butyl) cyclohexanol acetate,
(4-OH-4-Me-2-) pentanone, octanol acetate,
(n-) pentadecanol, benzaldehyde)
Severe (methyl salicylate, hexacosane, (1-)
tetradecene, docosane, ethylhexanol)
FAIMS: Field asymmetric ion mobility spectrometry; GC-DMS: Gas chromatography-differential mobility spectrometry; HLB: Huanglongbing.
Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004
7
peppermint). The NTD-IMS measured a-pinene concentration of
43 ng/mL in pinus species and MESI-IMS measured a-pinene con-
centration of 2.3 ng/mL in peppermint. Overall, the above litera-
tures suggest prospective of the IMS based VOC monitoring
technologies for overall plant health monitoring.
3.4. Evaluating produce quality
Quality attributes of fresh and stored agricultural produce
(freshness, taste/flavour) play a significant role in consumer
acceptance of the product and marketability (Govindasamy et al.,
1997). Traditional quality evaluation involves manual assessment,
which can be time consuming, laborious, less efficient, and may
involve in consistencies. Moreover, available analytical techniques
such as GC/MS do not allow simple real-time monitoring. An IMS
technology could be one alternative for the real-time monitoring of
the quality of agricultural produce. Some examples of use of IMS in
agricultural produce quality are listed in Table 4.
Potato industry is among the largest agricultural industry
worldwide. The potatoes rot during storage and can cause major
losses every year. Thus, it has become critical for maintaining the
health and quality of potatoes in bulk storages. When diseases such
as bacterial soft rots infect potatoes, it emits specific volatile com-
pounds such as ethylene, 1-propanol, and acetone (Bethke, 2012).
The recognization of these emitted volatile compounds can provide
opportunity for the initiation of early preventative steps in the
storage facilities. Several studies have shown the potency of the
VOCs profiling based technologies for disease detections in potato
(Kushalappa et al., 2002; Lui et al., 2005; Rutolo et al., 2014; Khot
et al., 2014). Monitoring of the potato quality (soft rot diseases
status) through gas analysis can be a potential method since
modern potato storage facilities are modulated with regular air
flow through potatoes to control the environment (Rutolo et al.,
2014).
Owlstone (2013) reported use of FAIMS technology (Lonestar,
Owlstone, UK) for disease detection in postharvest stored potato
and observed different volatile fingerprints from a healthy potato
tuber compared to that from an infected tuber. This indicates that
IMS technology can be useful in detecting soft rot and perhaps
other potato diseases in bulk storage. Similarly, Rutolo et al. (2014)
reported use of FAIMS technology (Lonestar, Owlstone, UK) to
Detection limit IMS type Study purpose Reference
ng/mL Portable Sabre 2000- Detect a-pinene emitted Wu, 2009
IMS(Smiths Detection, from plants
Mississauga, ON, Canada)
e Portable FAIMS (Lonestar, Detect powdery mildew Zhang et al., 2011
Owlstone Nanotech Ltd., and spider mites on tomato
Cambridge, UK) plants
e Portable GC-DMS (custom Detect citrus Aksenov et al., 2014
made) Huanglongbing disease
8 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12

Table 4
Typical IMS applications in agriculture produce quality.

Sample Target analytes Detection IMS used Study purpose Reference

limit

Apple, orange, and mixture of pesticides b-BHC, g-BHC, cis-chlordane, pg
trans-chlordane, endosulfan,
endrin ketone, parathion
Pistachio Aflatoxins B1 and B2
Different substances representing three commonly used Parathionmethyl, primicarb,
chemicals of pesticides (organophosphorous pesticides, promecarb, carbaryl,
pyrethroides and carbamates) in apples, grapes, tomatoes permethrin
and pepper
Potato tubers VOCs emitted from healthy
and infected potato tubers
GC-IMS (Barringer, GC- Detect pesticides on DeBono
IONSCAN with solid phase imported fruits et al.,
desorption (SPD) add on 2001
module)
ng CD-IMS using corona Quantitative Sheibani
discharge as ion source and determination of trace et al.,
N2 as carrier gas levels of aflatoxins in 2008
pistachio
ng UV laser desorption-DMS Rapid detection/ Borsdorf
(DMS from SIONEX screening of pesticides et al.,
Corporation, Bedford, USA) from fruit surfaces 2009
e Portable FAIMS (Lonestar, Detect soft rot disease Rutolo
Owlstone Nanotech Ltd., in stored potato tubers et al.,
Cambridge, UK) 2014

IMS: Ion mobility spectrometry; GC-IMS: Gas chromatography IMS; FAIMS: Field asymmetric ion mobility spectrometry; UV: Ultra-violet; CD-IMS: Corona discharge IMS;
VOCs: Volatile organic compounds.

detect disease (soft rot) in stored potatoes. Analysis of 156 samples
using PCA and k-means clustering showed differences in volatile
trends between diseased and control potatoes in all the experi-
ments (standard and early detections). Similarly, classification ac-
curacy up to 92% was obtained with linear discriminant analysis
during classification.
In the U.S., potato bulk storage losses average to about 7.5%
annually (Olsen et al., 2006). During curing and holding periods, the
infected tubers with favorable conditions may increase the storage
diseases severity and spread. Some key diseases that affect the
produce quality during storage are pink rot, pythium leak, late
blight, early blight, and soft rot or combination of these and other
diseases. Therefore, early disease detection of potato rots during
storage is critical to reduce the disease spread, and preventing
losses. Khot et al. (2014) evaluated feasibility of a handheld DMS
(Chemring Detection Systems Inc., NC) for VOCs biomarkers based
potato soft rot detection at early stages during postharvest storage.
The potato storage facilities from where the samples were collected
and sample storage condition during the temporal study are as
shown in Fig. 3.
Four replicate healthy and rotting Russet potato samples were
kept separately in eight identical 3.8 L glass jars and stored in a
humidity-controlled environment (4  C, 80e95% relative humidity)
before analysis. Each sample was analyzed twice on three separate
occasions (0, 2, and 5 weeks) to chart the different VOCs released
during the rot propagation process. During the non-contact anal-
ysis, DMS was positioned at the lip of the sample jars. Cell tem-
perature of the instrument was held constant at 50  C. System
background spectra were collected between the each sample
analysis. The spectra were collected in full scans across
400 Ve1000 V dispersion voltage (Vd) and 40 V to þ10 V
compensation voltage (Vc). Fig. 4 and Table 5 illustrates pertinent
results where DMS spectral based intensities were extracted at
specific Vc and Vd. Overall, DMS spectral signatures were different
in the detecting VOCs biomarkers of the healthy and the rotting
potato samples. The VdVc spectra displayed an increasing in-
tensity (Table 5) trend during the five-week storage of rotting
samples. Intensity peaks found at specific Vd and Vc can help with
identification of the different compounds and the type of rot.
In another study, Eiceman et al. (2013) summarized the appli-
cation of IMS for evaluating pesticide residues on the surfaces of
fruits and mycotoxins in nuts. Sample studies on the application of
IMS in detecting toxic materials in contaminated agricultural pro-
duce such as fruits and vegetables are listed in Table 4.
DeBono et al. (2001) detected pesticides residues on fruits such
as apples and oranges by solid phase desorption with a GC-IMS

Fig. 3. Potato bulk storage facility with a) and c) representing healthy and rotting potato regions from where the samples shown in b) and d) were collected for DMS based spectral
signature analysis (Khot et al., 2014).

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 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12 9

Fig. 4. DMS spectra of a) blank air, b) healthy and c) rotting potato samples during week-1 of five-week temporal analysis period (Khot et al., 2014).

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10 G.K. Kafle et al. / Engineering in Agriculture, Environment and Food xxx (2016) 1e12
Table 5
Differential mobile spectrometry based healthy and soft rot potato VOC concentration changes at specific Vd and Vc (Khot et al., 2014).
Vd (V) Vc (V) Peak intensity (mean ± SD)a (a. u.)
Healthy week 1
600 5.75 0.000 ± 0.008
650 7.75 0.000 ± 0.005
950 11.5 0.000 ± 0.001
VOC: Volatile organic compound; Vd: dispersion voltage; Vc: Compensation voltage.
a
Average of 16 spectra’s (i.e. 4 replicates
4 spectra/replicate).
(with 63Ni ionization source). The pesticides in the samples were
identified based on their specific reduced mobility and GC retention
time. The pesticides mixture of seven different varieties (such as g-
BHC, b-BHC, trans-chlordane, cis-chlordane, endosulfan, parathion,
and endrin ketone) were also detected with limits of detection of
10e300 pg in negative ion mode. In another IMS study, Borsdorf
et al. (2009) investigated the general capability of laser
desorption-DMS technology for the rapid screening of pesticides
from fruit surfaces and detected most of the targets at positive ion
mode. Tests were conducted on apples, tomatoes, red peppers and
grapes obtained from biological cultivation (not sprayed with
pesticides). For contaminating the fruit samples, pesticides were
added to a small piece of fruit skin from each sample. These
contaminated samples were used for the analysis process. Distinct
pesticide peaks at different concentrations were observed. Overall,
due to possibility of rapid detecting of toxic chemicals, IMS tech-
nology could also be well adopted for screening imported/exported
fruits and vegetables.
3.5. Other pertinent applications
Food and beverage quality and safety assessment such as food
freshness and flavor monitoring, contaminants in food, and
detection of melamine in milk using IMS is another area of appli-
cation in agriculture (Karpas, 2013). Armenta et al. (2011) reported
that IMS can be ideal for meat quality monitoring. Similarly, Karpas
(2013) reported that IMS application in product classification and
identifying food adulteration is another rapidly growing field.
Some studies have also reported the application of IMS in the
wood industry. Bacterial and fungal growth in wood products can
be easily detected by monitoring the VOCs emitted from their
surface (Korpia et al., 1998; Ewen et al., 2004; Hübert et al., 2011;
Eiceman et al., 2013) to prevent losses in the wood industry.
Vautz et al. (2004b) used UV-IMS attached with MCC for detecting
acetone and octane in pine wooden surface. It was reported that
MCC made IMS optimally competent for the rapid identification of
VOCs under ambient conditions. Similarly, Schumann et al. (2012)
used FAIMS connected with GC for the identification of VOCs
from wooden panel (formaldehyde and other VOCs). Samples
recovered from the headspace of specimens (built using wood
panels) were pre-concentrated using conventional SPME and
thermally desorbed in a split/splitless GC injector. In earlier studies,
IMS was used to examine wood specimens to distinguish between
various wood trees species, determine bacterial infection, differ-
entiate between wood of different tree species, identify bacterial
infection, and determine the occurrence of solvents and penta-
chlorophenol (Voß et al., 1994; Vautz et al., 2004b).
4. Summary and future research thruts
The state of IMS technology and applications in agriculture are
reviewed in the present paper. IMS selectivity varies greatly with
ionization source, ion polarity, and degree of ion separation. High
Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
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Soft rot week 1 Soft rot week 2 Soft rot week 5
0.000 ± 0.021 0.051 ± 0.013 0.096 ± 0.042
0.024 ± 0.031 0.035 ± 0.010 0.104 ± 0.011
0.000 ± 0.001 0.004 ± 0.002 0.006 ± 0.009
sensitivity/selectivity, portability, and the possibility for real time
monitoring make IMS a potentially useful technology for applica-
tion in the different fields of agriculture. Overall, previous studies
showed good performance of IMS technology in sensing chemicals
released from soil, plant, and agriculture produce.
Low-cost and portable IMS technologies with well-established
techniques are needed for their broader applications in agricul-
ture. One of the limitations of many commercial IMS instruments is
the use of nitrogen as carrier gas, which can increase the cost of
operation and limit the real time applications. Improvements to
allow use of air as carrier gas with high selectivity and sensitivity
can be useful.
In general, previous studies recommend positive ion mode for
the plant volatile measurements during IMS operation. More
research is needed to validate these findings, and utilizing of FAIMS
or DMS technologies to simultaneously detect VOCs in positive and
negative ion mode, could be effective in agricultural applications.
Overall, further field-based studies are needed for effective evalu-
ation and development of IMS instruments for specific agricultural
applications. In addition, development of IMS technology for real
time monitoring can be beneficial for wider agricultural
applications.
Acknowledgement
This activity was funded, in part, by USDA National Institute for
Food and Agriculture, Hatch Projects WNP00745 and WNP00821.
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Please cite this article in press as: Kafle, G.K., et al., State of ion mobility spectrometry and applications in agriculture: A review, Engineering in
Agriculture, Environment and Food (2016), http://dx.doi.org/10.1016/j.eaef.2016.05.004