Chromatographia (2016) 79:285–291
DOI 10.1007/s10337-016-3022-3
ORIGINAL
Alternative Liquid–Liquid Microextraction as Cleanup
for Determination of Neonicotinoid Pesticides Prior
HPLC Analysis
Jitlada Vichapong1 · Rodjana Burakham2 · Supalax Srijaranai2 
Received: 14 August 2015 / Revised: 12 November 2015 / Accepted: 21 December 2015 / Published online: 18 January 2016
© Springer-Verlag Berlin Heidelberg 2016
Abstract  A simple microextraction, namely low-density
solvent with low-toxicity organic solvent-based dispersive
liquid–liquid microextraction (LDS-DLLME) and modi-
fied QuEChERS sample preparation procedures were opti-
mized and validated for preconcentration of neonicotinoid
pesticides prior to the determination using HPLC. The
experimental parameters affecting the extraction efficiency,
including salt addition, type of disperser solvent and its
volume, effect of extraction solvent and its volume, and
extraction time were investigated. Under the selected LDS-
DLLME and HPLC conditions, separation of seven neonic-
otinoid pesticides (imidacloprid, acetamiprid, clothianidin,
thiacloprid, thiamethoxam, dinotefuran, and nitenpyram)
was achieved within 26 min. 1-Octanol (extraction solvent)
and acetonitrile (disperser solvent) were used for extrac-
tion of the target analytes. Under the optimum condition,
linearity was obtained within the range of 0.1–1000 ng g−1
with a correlation coefficient more than 0.999. The high
enrichment factor of the target analytes was 50-fold and
a low limit of quantitation (0.80–2.50 ng g−1) could be
obtained. The fruit samples (at fortified levels of 10, 30,
and 50 ng g−1) were successfully analyzed, and relative
recoveries were obtained in the range of 90.07–112.22 %.
* Jitlada Vichapong
jitlada.v@msu.ac.th; jitlada_v@yahoo.com
1
Creative Chemistry and Innovation Research Unit,
Department of Chemistry, Center of Excellence
for Innovation in Chemistry, Faculty of Science,
Mahasarakham University, Mahasarakham 44150, Thailand
2
Materials Chemistry Research Center, Department
of Chemistry, Center of Excellence for Innovation
in Chemistry, Faculty of Science, Khon Kaen University,
Khon Kaen 40002, Thailand
Keywords  Low-toxicity organic solvent-based dispersive
liquid–liquid microextraction · QuEChERS · Extraction ·
HPLC · Neonicotinoid pesticides
Introduction
Neonicotinoids have been the fastest growing class of
insecticides in modern crop protection [1]. There are seven
commercial neonicotinoids: imidacloprid, acetamiprid,
nitenpyram, thiacloprid, thiamethoxam, clothianidin and
dinotefuran. These insecticides are active against numerous
sucking and biting pests and insects, including whiteflies,
aphids, beetles and some lepidoptera species [2]. They act
as agonists at the insect nicotinic acetylcholine receptors
(nAChRs), which play an important role in synaptic trans-
mission in the central nervous system [3]. They can give
rise to serious risks for the health and safety of the consum-
ers of the agricultural products due to their distribution over
large areas of agricultural land [2]. Many countries have
formulated strict limits for neonicotinoids in various matri-
ces to ensure that the residues are below the safety limit for
maximum residue levels (MRLs). The MRLs of neonicoti-
noids range between 0.1 and 1 mg kg−1 [4].
Due to their low volatility and high polarity, neonicoti-
noid insecticides are unsuitable for direct analysis by gas
chromatography [5]. Nowadays, high-performance liquid
chromatography (HPLC) coupled with various detection
systems, including electrochemical (ECD) [6], fluorescence
(FLD) [7], UV/diode array (DAD) [8, 9] and mass spec-
trometry [10], is the favored technique for multi-analysis of
neonicotinoid pesticides. Although a MS detector provides
more sensitivity and selectivity than UV for monitoring tar-
get compounds in complex samples, it suffers from being a
very expensive and complex instrument [11]. Due to their
13
286 J. Vichapong et al.

low concentrations and complex matrices in real sample CH3 HN NO2

N
analysis, sample preparation is another step still required C N
N N N
before analysis. CH3
Cl N Cl N
Sample clean-up techniques are the most commonly
Acetamiprid Imidacloprid
employed, which comprise liquid–liquid extraction (LLE)
[12], solid-phase extraction (SPE) [13, 14], combinations
N NO2
of LLE and SPE [3, 15, 16], accelerated solvent extraction H H
N N N
(ASE) [17], quick, easy, cheap, effective, rugged, and safe Cl S NO2
(QuEChERS) [18], and dispersive liquid–liquid microex- N O N N
H H
traction (DLLME) [19, 20]. DLLME is based on the for- Clothianidin Dinotefuran
mation of fine droplets of an extractant in an aqueous sam-
ple solution when a water-immiscible extraction solvent Cl N NO2
(extractant) dissolved in a water-miscible organic dispersive N N
N N
solvent is rapidly injected into the aqueous sample solution NO2
[2]. The analytes in the sample solution are extracted into HN
O N Cl
S
the fine droplets, which are further separated by centrifu- Nitenpyram Thiamethoxam
gation, and the enriched analytes in the sedimented phase
are then analysised. The main advantages of the DLLME N
N
include simple operation, low cost, speed, high preconcen-
tration factors, and the use of small volumes of solvents N
S
[10]. On the other hand, the disadvantages of the DLLME Cl N
are its relatively low selectivity towards target analytes and Thiacloprid

the use of chlorinated solvents (e.g., chloroform, dichlo-

romethane, carbon tetrachloride) which pose a potential
threat to the environment [20]. In 2008, Leong and Huang
[21] developed a dispersive liquid–liquid microextraction
method based on solidification of floating organic droplets
(DLLME-SFO). In DLLME-SFO, solvents with densities
lower than water with a low-toxicity organic solvent are
required. The large contact surface between the sample and
the droplets of the extraction solvent speeds up mass trans-
fer, as rapidly as DLLME and with a shorter extraction time
than liquid–liquid microextraction based on solidification of
floating organic droplets (LLME-SFO). DLLME-SFO was
developed for the determination of organic pollutant [22],
amphetamines [23], triazine herbicides [24], and policyclic
aromatic hydrocarbons [25].
The aim of the present work was to develop a simple
low-density solvent with a low-toxicity organic solvent-
based DLLME and modified QuEChERS sample prepa-
ration procedures for the preconcentration and simulta-
neous analysis of neonicotinoid insecticide residues (i.e.
imidacloprid, acetamiprid, nitenpyram, thiacloprid, thia-
methoxam, clothianidin and dinotefuran) prior to HPLC
analysis. The effect of the experimental parameters on the
extraction performance of the target analytes, such as salt
addition, type and volume of extraction solvent, type and
volume of disperser solvent and centrifugation time were
investigated and optimized. The method was demonstrated
to apply to the analysis of fruit samples.
Fig. 1  Chemical structures of the studied neonicotinoid pesticides
Experimental
Chemicals and Reagents
All chemicals used were of at least analytical reagent
grade. The chemical structures of the studied neonicoti-
noids evaluated here are shown in Fig. 1. The analytical
standards of neonicotinoid insecticides including acetami-
prid, clotianidin, nitenpyram, imidacloprid, and thiameth-
oxam were obtained from Dr. Ehren-storfer (Germany),
and dinotefuran and thiacloprid were obtained from
Sigma-Aldrich (Germany). The stock solutions of each
insecticide were prepared at 1000 mg L−1 by dissolving
an appropriate amount in methanol (MeOH). Deionized
water obtained from RiOsTM Type I Simplicity 185 (Mil-
lipore Waters, USA) with a resistivity of 18.2 MΩ cm
was used throughout the experiments. Methanol (MeOH)
and acetonitrile (ACN) of HPLC grade and acetone were
obtained from Merck (Germany). Ethanol was purchased
from RCI Labscan (Thailand). NaCl and anhydrous
Na2SO4 were obtained from Ajax Finechem (New Zea-
land), CH3COONa and KI were obtained from Carlo Erba
(France).

13
Alternative Liquid–Liquid Microextraction as Cleanup…
Apparatus
The HPLC system comprised of a Waters 600 multisolvent
delivery system (USA), a Rheodyne injector with a sample
loop of 20 µL, and a Waters 996 photodiode array detector.
The Millennium software was used was utilized to control.
An Atlantis dC18 (4.6 × 150 mm, 5.0 µm) column (Waters,
USA) was used for separation of the target neonicotinoids.
Fruit Samples Analysis
Fruit samples including watermelon, longan and grape were
randomly purchased from local markets in Mahasarakham
province, northeast Thailand. The edible parts of the fruit
samples (500 g) were cut and blended using a commercial
food mixer. A modified QuEChERS method [26, 27] was
applied for sample preparation of the studied fruit sam-
ples. Briefly, the procedure was as follows: 10 g of sample
was placed in a 50-mL centrifugation tube and mixed with
20 mL of 1 % (v/v) acetic acid in ACN, and the mixture
vortexed for 1 min. After that, anhydrous Na2SO4 (15 g)
and sodium acetate (1 g) were added and the mixture was
immediately shaken manually. The solution was then cen-
trifuged at 3000 rpm for 5 min. The supernatant was sub-
sequently evaporated to dryness using a rotary evaporator
(40 °C water bath). The resulting residue was re-dissolved
with 10.00 mL of water before extraction by a low-density
solvent with low-toxicity organic solvent-based dispersive
liquid–liquid microextraction procedure.
Low Density Solvent with Low‑Toxicity Organic
Solvent‑Based Dispersive Liquid–Liquid
Microextraction Procedure (LDS‑DLLME Procedure)
A 10-mL aliquot of sample (or standard solution) was mixed
with 2.5 g of Na2SO4 and then subsequently transferring to
a 10-mL screwcap test tube. After that, a mixture of 100 µL
extraction solvent (1-octanol) and 50 µL dispersive solvent
(acetonitrile) were injected rapidly into the sample solution.
A cloudy solution because of the dispersion of 1-octanol in
the solution was obtained. After that, the resulting emulsion
was completely separated by centrifugation at 3500 rpm for
10 min. The reconstituted solution floated on the top of the
tube. The upper extraction solvent was collected by a 1-mL
syringe and then injected into the HPLC for analysis.
Results and Discussion
Chromatographic Analysis
The simultaneous separation of the studied neonicotinoids
was carried out on a reversed-phase HPLC system with
287
the isocratic elution using 25 % (v/v) acetonitrile in water
at a flow rate of 1.0 mL min−1. The injection volume was
20 µL. The detection of the target analytes was set at the
maximum absorption wavelength of 254 nm. Seven neo-
nicotinoid insecticides were separated within 25 min with
the elution order of dinotefuran (tR = 2.74 min), nitenpyran
(tR = 2.98 min), thiamethoxam (tR = 6.81 min), clothiani-
din (tR = 9.51 min), imidacloprid (tR = 11.45 min), aceta-
miprid (tR = 14.01 min) and thiacloprid (tR = 24.31 min).
Optimization of LDS‑DLLME Procedure
In order to obtain the high extraction efficiency of the pro-
posed LDS-DLLME method, several factors were investi-
gated including salt addition, the type of disperser solvent
and its volume, the type of extraction solvent and its vol-
ume, and the extraction time. The optimization was car-
ried out on the aqueous solution (10.00 mL) containing
500 ng g−1 of each analyte. All the experiments were per-
formed in triplicate and the mean of the results were used
for optimization.
Generally, the addition of salt decreases the solubility of
analytes in aqueous samples and enhances their distribution
into the organic phase [28]. In this experiment, 1 g of NaCl,
Na2SO4, CH3COONa were investigated and the results were
compared with that obtained from the process without salt
addition (data not shown). It was found that the addition
of Na2SO4 provided higher extraction efficiency in term of
peak area of neonicotinoids. Therefore, the concentration
of Na2SO4 on the extraction efficiency of the target neoni-
cotinoid analytes were also studied within the range of 0.5–
4.0 g. The results in Fig. 2 show an enhancement of extrac-
tion efficiency for all neonicotinoids when 2.5 g Na2SO4 was
added. Salt solutions reached or exceeded their solubility
900000 Dinotefuran
Nitenpyram
Thiamethoxam
750000 Clothianidin
Imidacloprid
Acetamiprid
600000 Thiacloprid
Peak area
450000
300000
150000
0
0.0 0.5 1.0 1.5 2.0 2.5
Concentration of Na2SO4 (g)
Fig. 2  Effect of concentration of salt on the extraction of neonicoti-
noids
13
288 J. Vichapong et al.

limits when the amount of salt was more than 2.5 g. There-
fore, 2.5 g Na2SO4 was selected for further studies.
In LDS-DLLME, the dispersive solvent is one of the
most important factors that accelerates the emulsification of
water-immiscible extraction solvent affecting the extraction
efficiency. For the investigation, various types of disperser
solvent (50 µL) including acetonitrile, methanol and etha-
nol were studied. As shown in Fig. 3a, the results showed
that acetonitrile gave a higher extraction efficiency in term
of peak area compared to ethanol and methanol; therefore,
it was selected as the disperser solvent.
To investigate the effect of the disperser solvent (ace-
tonitrile) volume on the extraction efficiency, several vol-
umes of acetonitrile in the range of 25–250 µL were studied
(Fig. 3b). It was found that, if the disperser solvent volume
is 25 µL, the solution cannot complete phase separation. It
was noted that a disperser solvent volume of 50 µL provide
because 1-octanol has a lowrt density than other extraction
solvents (data not shown). Consequently, 1-octanol was
selected as the extraction solvent for further study.
The effect of extraction solvent volume was studied for
1-octanol volume in the range from 50 to 750 µL. It was
found that when the extraction solvent volume is 50 µL, the
solution cannot complete phase separation. Moreover, the
extraction solvent volume of more than 100 µL decreased
the peak area of neonicotinoids. As can be seen from Fig. 4,
the highest extraction efficiency was obtained using 100 µL
of 1-octanol. Therefore, 100 µL of 1-octanol was selected
for further study.
Centrifugation time is another important step in LDS-
DLLME for achieving phase separation. Therefore, the
effect of centrifugation time was studied in the range of
1–15 min at 3500 rpm. It was found that the peak areas
of all analytes increased by applying centrifugation up to

Dinotefuran Dinotefuran
Nitenpyram
a 1200000
Nitenpyran
Thiamethoxam
b 900000 Thiamethoxam
Clothianidin Clothianidin
1000000 Imidacloprid 750000 Imidacloprid
Acetamiprid Acetamiprid
Thiacloprid Thiacloprid
800000 600000
Peak area

Peak area

600000 450000

400000 300000

200000 150000

0 0
Ethanol Acetonitrile Methanol 0 50 100 150 200 250
Kind of disperser solvent Volume of acetonitrile (µL)

Fig. 3  Effect of a the kind of disperser solvent and b the volume of extraction solvent on the extraction of neonicotinoids

the highest peak area. Therefore, acetonitrile 50 µL was Dinotefuran

1400000
selected for further study. Nitenpyram
Thiamethoxam
In the LDS-DLLME method, extraction solvents have 1200000
Clothianidin
to be low-toxicity solvents and these solvents have to fulfill Imidacloprid
1000000
some requirements such as low density compared to water, Acetamiprid
Thiacloprid
Peak area

low solubility in water and have a proper melting point as 800000

well as the other requirements that are available in each
600000
solvent, such as high extraction capability for target com-
pounds, good chromatographic behavior, cheap, low vola- 400000
tility to minimize solvent losses during extraction and high
purity [24]. Based on these requirements for the extraction 200000

solvent, four types of low-density organic solvent were 0

investigated (data not shown) including 1-octanol [density 100 125 150 175 200 225 250
(d) = 0.8240 g mL−1], 1-dodecanol (d = 0.8309 g mL−1), Volume of 1-octanol (µL)
toluene (d  = 0.8700 g mL−1), and ethyl acetate
(d = 0.8970 g mL−1). It is clearly seen that 1-octanol pro- Fig. 4  Effect of volume of 1-octanol on the extraction of neonicoti-
vided a high extraction efficiency in terms of peak area noids

13
Alternative Liquid–Liquid Microextraction as Cleanup… 289

10 min, and then gradually decreased. Consequently, a cen-
trifugation time of 10 min was selected.
Analytical Performance of the Method
Under the above-mentioned conditions, the proposed LDS-
DLLME combined with the HPLC method for the determi-
nation of neonicotinoid pesticides was validated by deter-
mining its analytical characteristics, i.e. linearity, precision,
limit of detection (LOD), limit of quantitation (LOQ) and
enrichment factor. The analytical performances of the pro-
posed method are summarized in Table 1. The calibration
curves of all the analytes were linear in the range from 0.1
to 1000 ng g−1 with a correlation coefficient (R2) more than
0.999. The enrichment factors, defined as the concentration
ratio of the analytes in the settled phase (Cset) and in the
aqueous sample (Co), were 50 for all compounds. The chro-
matograms obtained from the separation of standard neo-
nicotinoids by HPLC without and with the LDS-DLLME
procedure are compared in Fig. 5a and b, respectively. The
LOD and LOQ were determined based on the concentra-
tion giving a signal-to-noise ratio of 3 (S/N  = 3) and 10
(S/N  = 10), respectively. LOD were found to be in the
range of 0.25–0.80 ng g−1 and LOQ in the range of 0.80–
2.50 ng g−1. The RSDs of five consecutive extractions of
the standard solution containing 50 µg kg−1 nenonicoti-
noids were in the ranges of 0.52–1.97 and 2.59–6.38 % for
retention time and peak area, respectively.

Table 1  Analytical performances of the proposed method

Insecticide Linear equation Linearity (ng g−1) r2 LOD (ng g−1) LOQ (ng g−1) %RSD EF
tR Peak area

Dinotefuran y = 167,991x − 516 0.1–1000 0.9998 0.80 (100)a 2.50 0.52 5.30 50

Nitenpyram y = 169,284x − 612 0.1–1000 0.9998 0.80 (100)a 2.50 0.83 4.18 50
a
Thiamethoxam y = 469,542x − 2324 0.1–1000 0.9994 0.40 (60) 1.20 1.45 2.59 50
Clothianidin y = 1,000,000x − 1001 0.1–1000 0.9995 0.25 (50)a 0.80 1.62 3.06 50
Imidacloprid y = 891,512x − 5835 0.1–1000 0.9997 0.30 (60)a 1.00 1.35 2.85 50
Acetamiprid y = 2,000,000x − 43,547 0.1–1000 0.9997 0.25 (50)a 0.80 1.58 5.15 50
Thiacloprid y = 2,000,000x + 20,910 0.1–1000 0.9997 0.25 (50)a 0.80 1.97 6.38 50

LOD limit of detection in ng g−1, LOQ limit of quantitation in ng g−1, RSD relative standard deviation (n = 5), EF enrichment factor
a
  Values reported in parentheses obtained from the standard neonicotinoids without preconcentration (direct injection)

Fig. 5  Chromatograms of 6
standard neonicotinoids: a 0.040
4
without LDS-DLLME and b
with LDS-DLLME; concen- 0.035
tration of all standards was 5
500 ng g−1. Peak assignments: 7
1 dinotefuran, 2 nitenpyran, 3 0.030
thiamethoxam, 4 clothianidin, 5 3
Voltage (mV)

imidacloprid, 6 acetamiprid and 0.025

7 thiacloprid
1
0.020
2

0.015

0.010
(b)
0.005 1
3
2 4 5 6
7 (a)
0.000

0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 21.00 22.00 24.00 26.00 28.00
Time (min)

13
290 J. Vichapong et al.

Table 2  Recovery of the studied neonicotinoids spiked in fruit samples obtained by the proposed method
Analyte Spiked (ng g−1) Watermelon (n = 3) Longan (n = 3) Grape (n = 3)
Recovery (%) RSD (%) Recovery (%) RSD (%) Recovery (%) RSD (%)

Dinotefuran 0 – – – – – –
10 102.78 2.02 98.93 2.54 92.60 3.66
30 98.82 0.78 97.82 2.54 98.93 1.82
50 110.53 0.81 95.28 0.67 90.07 0.10
Nitenpyram 0 – – – – – –
10 94.90 0.75 93.47 2.35 92.97 2.26
30 98.89 2.26 97.72 1.51 100.64 3.21
50 93.79 0.90 99.32 1.79 101.52 0.34
Thiamethoxam 0 – – – – – –
10 97.60 1.42 93.27 2.61 105.60 3.34
30 96.78 0.84 91.78 1.50 104.89 1.73
50 99.25 1.03 100.49 1.12 102.69 1.08
Clothianidin 0 – – – – – –
10 104.75 0.45 100.03 1.30 99.70 1.40
30 97.78 1.49 97.78 1.49 107.78 2.12
50 99.69 2.13 101.02 1.10 105.35 1.20
Imidacloprid 0 – – – – – –
10 104.03 1.25 102.37 3.46 103.37 3.73
30 112.22 2.38 100.22 2.93 102.11 1.50
50 110.69 2.09 99.82 0.33 100.62 1.00
Acetamiprid 0 – – – – – –
10 107.75 2.83 97.70 2.33 97.03 3.03
30 93.22 1.79 99.78 0.33 102.33 2.11
50 91.69 1.95 100.22 0.43 100.09 0.09
Thiacloprid 0 – – – – – –
10 101.7 2.53 105.7 1.82 100.37 4.26
30 93.67 0.51 101.11 0.77 102.33 1.92
50 99.42 1.16 108.69 1.12 100.22 0.63

– not detected

Application to Real Fruit Samples Conclusions

The proposed LDS-DLLME procedure was applied for the
determination of neonicotinoid pesticides in fruit samples to
elucidate the applicability and reliability of this method. In
this study, no residues of the neonicotinoids were detected
in the samples (Table 2). In order to validate the accuracy
of the established method, fruit samples were spiked with
neonicotinoid pesticides at concentration levels of 10, 30,
and 50 ng g−1. As indicated in Table 2, the recoveries of the
studied neonicotinoid pesticides were between 90.07 and
112.22 % with RSDs of less than 4.26 %. Good recoveries
were obtained, indicating that the performance of the method
was not affected by the sample co-extractives, at least for the
matrices studied in this work. Figure 6 shows a typical chro-
matogram of watermelon and spiked watermelon samples
using the LDS-DLLME procedure and HPLC analysis.
A simple miniaturized extraction method, namely low-
density solvent with a low-toxicity organic solvent-based
dispersive liquid–liquid microextraction (LDS-DLLME)
and a modified QuEChERS method was developed for the
extraction and preconcentration of seven neonicotinoid pes-
ticides in fruit samples before their analysis by HPLC. The
proposed extraction method is simple, fast and effective
and convenient in operation. The developed method shows
good analytical features providing low limits of detection
at the level of 0.25–0.80 ng g−1 which is below the accept-
able MRLs for neonicotinoids. High preconcentration fac-
tors, good recoveries and high reproducibility were also
obtained. The proposed method has the potential to be used
as an alternative green extraction method for the determina-
tion of neonicotinoids in fruit samples.

13
Alternative Liquid–Liquid Microextraction as Cleanup… 291

Fig. 6  Chromatograms of a
0.10
watermelon and b watermelon
spiked with 100 ng g−1 of each
neonicotinoid. Peak assign-
ments are described in Fig. 5 0.08

0.06

Voltage (mV)
0.04

1 3 4
0.02 2 6 7
5
(b)
0.00

- 0.02 (a)

0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 21.00 22.00 24.00 26.00 28.00

Time (min)

Acknowledgments  This article is dedicated to Professor Dr. Kate
Grudpan (Chiang Mai University, Thailand) in celebration of his 60th
birthday. The authors gratefully acknowledge the financial supports
of this research by the Thailand Research Fund (TRF) and Mahasara-
kham University, through the TRF Grant for New Scholars (Grant no.
TRG5780060). The authors also gratefully acknowledge the partial
supports for this research from the Center for Innovation in Chem-
istry (PERCH-CIC), Commission on Higher Education, Ministry of
Education, and Materials Chemistry Research Center, Khon Kaen
University.
Compliance with Ethical Standards  Frenich AG, Vidal JL (2011) Talanta 85:183–196
Conflict of Interest  The authors declare that they have no conflict
of interest.
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