Food Control 110 (2020) 106982

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Food Control
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Occurrence of deoxynivalenol and zearalenone in cereals and cereal T

products from Turkey
Ozgur Golgea, Bulent Kabakb,∗
a
Alanya Alaaddin Keykubat University, Faculty of Tourism, Department of Gastronomy and Culinary Arts, Alanya, Antalya, Turkey
b
Hitit University, Faculty of Engineering, Department of Food Engineering, TR-19030, Corum, Turkey

A R T I C LE I N FO A B S T R A C T

Keywords: This report describes concentrations of deoxynivalenol (DON) and zearalenone (ZEA) in cereals and derived
Deoxynivalenol products collected in Turkey from 2015 to 2018. A total of 240 cereals and cereal products were analysed by
Zearalenone high performance liquid chromatography coupled with photodiode array (HPLC-PDA) and fluorescence (HPLC-
Cereal quality FLD) detectors. The analytical method performance was satisfactory, with limit of quantification (LOQ) values of
Occurrence
46.90–72.30 μg kg−1, and 3.50–3.70 μg kg−1 for DON and ZEA, respectively. Thirteen wheat (58–1092 μg kg−1),
Food safety
HPLC
two maize (313–331 μg kg−1), three barley (138–973 μg kg−1), seven paddy rice (136–256 μg kg−1), three
wheat flour (92–151 μg kg−1), two biscuits (31.2–71.3 μg kg−1) and only one pasta (49.3 μg kg−1) contained
Chemical compounds studied in this article: DON, but levels were below the EU maximum level (ML). DON was not detected in bulgur and wheat bread. ZEA
Deoxynivalenol was found in two wheat, three maize, eleven paddy rice and two wheat flour with a mean middle bound ZEA
PubChem CID: 40024 level of 1.34, 28.0, 42.9, and 2.66 μg kg−1, respectively. Amongst the samples contaminated with ZEA, only one
Zearalenone paddy rice exceeded EU ML of 100 μg kg−1. However, barley, bulgur, wheat bread, pasta and biscuit products
PubChem CID: 5281576 did not contain ZEA.

1. Introduction which are frequently observed in temperate regions of Europe (EFSA,

Mycotoxins are naturally occurring compounds produced by fila-
mentous fungi in many agricultural products but especially in oilseeds,
nuts, dried fruits and cereal grains both in the field and during storage.
While the mycotoxin contamination is a world-wide problem, these
chemicals occur mainly in regions with climates of high humidity and
temperature or where there are poor storage conditions. Within the
over 300 mycotoxins identified, the most commonly occurring ones in
nature are aflatoxins (AFs), ochratoxin A (OTA), patulin (PAT) and
Fusarium toxins such as fumonisins (FBs), T-2/HT-2 toxins, deox-
ynivalenol (DON) and zearalenone (ZEA) (Sweeney & Dobson, 1998).
DON (also known as vomitoxin) and ZEA are produced by Fusarium
species and occur mainly in cereal grains such as wheat and maize as
well as cereal-based foods and feedstuffs. DON, a member of the largest
group of sesquiterpene fungal metabolites named trichothecenes, is
most prevalent among Fusarium toxins and an important indicator of
the occurrence of Fusarium Head Blight (FHB) in wheat. DON is pro-
duced predominantly by Fusarium graminearum and Fusarium culmorum,
2013). Wheat is the predominant source of exposure to DON in most
diets. Following exposure with a high acute dose, DON can induce
gastrointestinal symptoms such as vomiting both in humans and ani-
mals. In long term exposure, this compound can lead to weight gain
suppression and anorexia in animals. The provisional maximum toler-
able daily intake (PMTDI) of 1 μg kg−1 body weight (b.w.) and acute
reference dose (ARfD) of 8 μg kg−1 b.w. day−1 for DON and its meta-
bolites have been established by the Joint FAO/WHO Expert Committee
on Food Additives (JECFA) (EFSA, 2017).
ZEA is an oestrogenic mycotoxin that is co-produced with DON
primarily by Fusarium graminearum and Fusarium culmorum. This com-
pound also synthesised by Fusarium cerealis, Fusarium equiseti, Fusarium
semitectum and Fusarium moniliforme. Although maize and maize-based
products are considered to be the main source of exposure to ZEA, the
toxin may also occur in other cereals such as barley, wheat, oat, rice
and sorghum in warm and temperate climate (EFSA, 2004). ZEA has
been associated with hyperoestrogenism in livestock, especially pig
characterised by vulvar and mammary swelling and reduced fertility.

Abbreviations: DON, deoxynivalenol; ZEA, zearalenone; HPLC-PDA, high performance liquid chromatography-photodiode array detector; HPLC-FLD, high per-
formance liquid chromatography-fluorescence detector; IAC, immunoaffinity column; LB, lower bound; LOD, limit of detection; LOQ, limit of quantification; MB,
middle bound; ML, maximum level; RSD, relative standard deviation; UB, upper bound
∗
Corresponding author.
E-mail address: bulentkabak@hitit.edu.tr (B. Kabak).

https://doi.org/10.1016/j.foodcont.2019.106982
Received 20 September 2019; Received in revised form 1 November 2019; Accepted 2 November 2019
Available online 05 November 2019
0956-7135/ © 2019 Elsevier Ltd. All rights reserved.
O. Golge and B. Kabak
Because of its toxicity, in 2011, the EFSA's CONTAM Panel established a
tolerable daily intake (TDI) of 0.25 μg kg−1 b.w. for ZEA (EFSA, 2011).
The carcinogenic potential of mycotoxins has been evaluated by In-
ternational Agency for Research on Cancer (IARC), and DON and ZEA
were placed in Group 3 (not classifiable as to their carcinogenicity to
humans) (IARC, 1993). The maximum levels (MLs) for mycotoxins,
including DON and ZEA in certain food products are laid down in
Commission Regulation 1881/2006 (European Commission, 2006b),
which is amended with Commission Regulation 1126/2007 to revise
MLs for Fusarium toxins in maize and maize products (European
Commission, 2007).
DON and ZEA contamination mostly caused by pre-harvest con-
tamination of cereals by Fusarium spp., but may also occur in storage if
the crop is not handled and dried properly or re-wetting of the crop
from condensation or rain. The major contributors to exposure of
Fusarium toxins are cereal derived products, in particular wheat and
maize-based. Due to mycotoxins are highly heat-stable and cannot be
readily destroyed by conventional heat processing, the toxin may also
be found in bread, bakery products, flour and products thereof.
There are many reports on AFs and OTA contamination in cereals
including wheat, maize and rice cultivated in Turkey. However, there is
little data about DON and ZEA content of mainly cultivated cereals and
their derived products in Turkey. Therefore, the main aim of this study
is to determine DON and ZEA contamination in cereals and cereal
products collected from Turkey, using high performance liquid chro-
matography (HPLC).
2. Materials and methods
2.1. Samples
In Turkey, a total of 240 samples of wheat (n = 50), maize (n = 15),
barley (n = 15), paddy rice (n = 20), wheat flour (n = 50), bulgur
(traditional processing wheat) (n = 10), wheat bread (n = 60), pasta
(n = 10) and biscuits (n = 10) were randomly collected from wholesale
places, grain-milling factories, retail market and supermarkets in
Antalya and Mersin provinces, Turkey between September 2015 and
August 2018. The sampling was conducted as described in the
Commission Regulation (EC) No 401/2006 (European Commission,
2006a). Due to possible inhomogeneous distribution of mycotoxins in
grains, the aggregate samples were milled with a laboratory mill (C.W.
Brabender Instruments, Inc., Germany) or homogenised using Waring
blender (Waring Products Co., Connecticut, USA) before analysis.
However, bread samples were sliced and dried at 50 °C in oven, then
grinding. Homogenised samples were stored at −18 °C until analysis.
2.2. Reagents and materials
Methanol and acetonitrile used were of HPLC-grade and were both
supplied from Sigma–Aldrich (St. Louis, MO, USA). Ultrapure water was
produced by a Milli Q water purification system (Millipore, Molsheim,
France). The immunoaffinity columns (IAC) DONPREP® and EASI-
EXTRACT® ZEARALENONE that contain monoclonal antibody specific
to the toxin and were supplied from R-Biopharm AG (Darmstadt,
Germany). The glassware and other items were washed with 5% sodium
hypochlorite solution, rinsed with water and dried before reusing.
Mycotoxin analytical standards (DON and ZEA) were purchased
from Sigma-Aldrich (St. Louis, MO, USA). From the crystalline stan-
dards (purities of ≥98%), individual stock solutions were prepared in
methanol and acetonitrile at concentrations of 100 μg ml−1 for DON
and 25 μg ml−1 for ZEA, respectively.
2.3. Sample extraction and IAC clean-up
DON and ZEA were extracted from samples according to the R-
Biopharm instruction manual, with slight modifications. Determination
2
Food Control 110 (2020) 106982
of DON is based on aqueous extraction, clean-up and enrichment by
means of IAC followed by HPLC detection. A ground sample of 25 g was
extracted with 200 ml water using a Waring blender for 3 min. The
sample extract was filtered through Whatman filter paper No.4. A 2 ml
of filtered extract was then passed through DONPREP® IAC at 1–2 drops
per second. The IAC was washed with 10 ml of phosphate buffered
saline (PBS) solution and 10 ml of ultrapure water, and dried with air.
DON was eluted from the IACs with 1.5 ml of methanol. The eluate was
concentrated to dryness under a nitrogen stream using a sample con-
centrator (50 °C) and reconstituted in 1 ml of methanol–water (15:85,
v/v).
ZEA was extracted from grain and cereal-based foods (25 g) with
125 ml acetonitrile–water (75:25, v/v) using Waring blender. 20 ml of
filtered extract was diluted with 80 ml PBS solution, and 25 ml of di-
luted extract was cleaned up by EASI-EXTRACT® ZEARALENONE. After
cleaning the IAC, ZEA was eluted by passing 1.5 ml of acetonitrile from
the IAC, 1.5 ml of water was then added and the mixture was trans-
ferred to an autosampler.
2.4. Chromatographic analysis
DON and ZEA were analysed with reversed phase HPLC coupled
with photodiode array (HPLC-PDA) (Thermo Scientific Accela HPLC
system, USA) and fluorescence detectors (HPLC-FLD) (Thermo
Scientific Dionex Ultimate 3000 HPLC system, USA), respectively.
Chromatographic separation was achieved using an Agilent ZORBAX
Eclipse C18 column (150 × 4.6 mm, 5 μm particle size). The column
temperature was set at 40 °C. DON analysis was performed with an
isocratic elution program using a mobile phase of methanol–water
(15:85, v/v) at a flow rate of 0.4 ml min−1 and the detection wave-
length was 220 nm. For ZEA analysis, the mobile phase consisting of
acetonitrile–water (52:48, v/v) was used in isocratic elution program
with a flow rate of 1 ml min−1. The fluorescence detector was operated
at excitation and emission wavelengths of 274 and 455 nm for the de-
tection of ZEA, respectively. The injection volumes were 100 μl and
20 μl for DON and ZEA analysis, respectively.
2.5. Method validation
The analytical methods of DON and ZEA were in-house validated in
terms of linearity range, method limits of detection and quantification
(LOD and LOQ), trueness (mean recovery), precision (repeatability and
within-laboratory reproducibility) and measurement uncertainty (MU).
Linearity over the intended working range (50–1000 μg l−1 for DON
and 2–500 μg l−1 for ZEA) was determined using a set of six calibration
standards, which were injected in triplicate. The standard curves were
plotted based on peak area versus analyte concentration.
Due to expected slight differences in matrix effects during HPLC
analysis and no differences in the sample extraction and IAC clean-up
procedure, wheat and maize samples were taken as blank materials for
validation study for both DON and ZEA. The LOD, LOQ, precision and
trueness were determined by fortified experiments using both wheat
and maize materials which were tested free from both DON and ZEA.
The LOD and LOQ values were measured by analysing 10 individual
blank wheat and maize samples fortified with 250 μg kg−1 for DON and
10 μg kg−1 for ZEA. The fortified samples were analysed as previously
described. The LOD and LOQ were calculated as 3 and 10 times the
standard deviation of replicate analyses (n = 10).
Method recovery and precision were assessed by recovery studies in
which both blank wheat and maize were fortified at two concentration
levels (500 and 750 μg kg−1 in wheat, and 825 and 1750 μg kg−1 in
maize for DON, and 50 and 100 μg kg−1 in wheat, and 175 and
350 μg kg−1 in maize for ZEA), corresponding to 0.5 and 1.0 times to
EU ML. Six replicates were prepared for each experiment. The repeat-
ability (intra-day precision, RSDr, n = 6) of the method was measured
on the same day by same operator, while within-laboratory
O. Golge and B. Kabak
reproducibility (inter-day precision, RSDR, n = 18) was determined on
three consecutive days with six replicates. The precision values were
expressed as relative standard deviation (%RSD) of replicate measure-
ments.
For the purposes of evaluating MU for the determination of DON
and ZEA in cereals, method performance characteristics were used and
combined in MU calculations. Based on EURACHEM Guidelines
(Ellison, Rosselin, & Williams, 2000), the standard combined un-
certainty (uc) was calculated using Eq. (1), by combining the individual
uncertainty associated with repeatability (u(RSDr)), within-laboratory
reproducibility (u(RSDWR)), mean recovery (u(bias)) and calibration
curve (uM).
2
uc = u (RSDr )2 + u (RSDwR)2 + u (bias )2 + uM (1)
The expanded uncertainty (U ′) was subsequently calculated by
multiplying uc, by a coverage factor (k) of two, which represents a 95%
confidence level.
3. Results and discussion
3.1. Validation data
The linearity, and method LOD and LOQ values for wheat and maize
matrices are presented in Table 1. The calibration curves were linear
over the working range of 50–1000 μg l−1 and 2–500 μg l−1 for DON
and ZEA, respectively. For both DON and ZEA, the coefficient of de-
terminations of linear functions (R2) were greater than 0.99. Suffi-
ciently low LODs and LOQs were obtained for both DON and ZEA in
wheat and maize matrices. The LOD values of DON and ZEA were 21.70
and 1.12 μg kg−1 in wheat, and 14.08 and 1.06 μg kg−1 in maize ma-
trices, respectively. The LOQs were in the range 46.90–72.30 μg kg−1
for DON, and 3.50–3.70 μg kg−1 for ZEA, which values are well below
the EU MLs and could be considered adequate for the evaluation of
these mycotoxins in cereals and cereal-by products.
Method recovery, precision and MU results were given in Table 2.
For both target analytes, good recoveries (85.8–98.6% for DON, and
97.4–105.1% for ZEA), repeatabilities (2.27–6.66% for DON, and
1.57–7.75% for ZEA) and within-laboratory reproducibilities
(2.17–5.46% for DON, and 2.30–6.48% for ZEA) were obtained, which
conformed to the requirements of Regulation EC 401/2006. There is
requiring recoveries of 60–110% and 70–120% for mass fractions
of > 100–≤ 500 μg kg−1, and > 500 μg kg−1, respectively, with RSDr
values of ≤20% and RSDR values of ≤40% for DON. The regulation
recommends recovery rate of 60–120% and 70–120%, with RSDr of
≤40% and ≤25%, and RSDR of ≤50% and ≤40% for mass factions of
≤50 and > 50 μg kg−1 for ZEA, respectively (European Commission,
2006a). The expanded measurement uncertainties were 16.3% for
DON, and 21.0% for ZEA. For both toxins, the obtained uncertainty
results associated with RSDr and RSDR represent the major sources of
the combined uncertainty.
3.2. Occurrence of DON and ZEA in cereals and cereal products
A summary of the DON and ZEA concentrations data is presented in
Table 3. In the analysis of data, the non-detects (left-censored data)
Table 1
The linearity, and method LOD and LOQ data.
Analyte Linearity
−1
Range (μg l ) Equation R 2
DON 50–1000 y = 1.099x–0.13 0.9999
ZEA 2–500 y = 12108x–369.4 0.9998
R2, coefficient of determination.
Food Control 110 (2020) 106982
were treated by the substitution method as described in the EFSA sci-
entific report (EFSA, 2010). Among the cereals and derived products,
the highest incidence of DON was detected in paddy rice (rice in the
husk), followed by wheat, barley and biscuits. Results below the LOD
accounted for 65% for paddy rice, 74% for wheat, 80% for both barley
and biscuits, 86.7% for maize, 90% for pasta and 94% for wheat flour,
while DON was not found in any of the wheat bread and bulgur sam-
ples. In wheat, barley, wheat flour, pasta and biscuits, DON was de-
tected relatively more frequently than ZEA. The highest mean con-
centration of DON was observed in wheat (LB = 112.6 μg kg−1;
UB = 128.6 μg kg−1), with concentrations ranging from 58 to
1092 μg kg−1. Barley had also a relatively high mean concentration of
DON (LB = 85 μg kg−1; UB = 102.4 μg kg−1), with the concentration at
the 95th percentile of 528.1 μg kg−1 and the maximum value of
973 μg kg−1. Compared to wheat and barley, maize had about two-fold
lower mean level of DON (LB = 42.9 μg kg−1; UB = 55.1 μg kg−1),
with a maximum measured value of 331 μg kg−1. The contamination
frequency (35%) was the highest in paddy rice, but the mean con-
centration was ranged from 68.4 μg kg−1 (LB) to 82.5 μg kg−1 (UB).
The mean DON concentration was recorded in wheat flour in the range
of 7 μg kg−1 (LB) to 27.4 μg kg−1 (UB), with a maximum concentration
of 151 μg kg−1. Mean DON values ranged from 10.3 μg kg−1 (LB) to
27.6 μg kg−1 (UB) for biscuits, and from 4.9 μg kg−1 (LB) to
24.5 μg kg−1 (UB) for pasta. The values for DON detected in cereals and
cereal products did not exceed respective EU ML.
Amongst the cereals and their products, paddy rice showed both the
highest frequency (55%) and mean concentration of ZEA
(LB = 42.6 μg kg−1; UB = 43.1 μg kg−1). However, only one paddy rice
sample exceeded the EU ML of 100 μg kg−1. ZEA was also co-occurred
with DON in 6 paddy rice samples at concentrations varying from 18.1
to 142 μg kg−1. The second-high frequency (20%) and mean con-
centration of ZEA (LB = 27.6 μg kg−1; UB = 28.5 μg kg−1) was ob-
served in maize. The co-occurrence of ZEA and DON was detected in
two maize samples. For paddy rice, the highest concentration was re-
corded as 256 μg kg−1, while for maize the highest reported ZEA level
was 337 μg kg−1. The left-censored data was recorded 96% for both
wheat and wheat flour. Both two wheat and wheat flour samples had
ZEA at levels 17.2 and 23 μg kg−1, and 51.6 and 54.6 μg kg−1, re-
spectively. None of the maize, wheat and wheat flour samples con-
tained ZEA at levels higher than EU ML. However, ZEA was absent in
barley, bulgur, wheat bread, pasta and biscuits products.
These values are much lower than previous observation by Gürsoy
and Biçici (2003) who detected DON and ZEA in 21.6% and 32% of 116
cereals (73 maize and 43 wheat) cultivated in Turkey, at levels varying
from 20 to 2540 μg kg−1, and from 36.2 to 627.6 μg kg−1, respectively.
Numanoglu, Uygun, Koksel, and Solfrizzo (2010) found DON and ZEA
in 80% and 70% of the 42 maize samples from Turkey, up to levels of
16100 μg kg−1 and 1600 μg kg−1, respectively. In another study, DON
was found in 13 out of 144 cereal and cereal-based products collected
from Istanbul, Turkey at levels varying from 132 to 9589 μg kg−1
(Bakırcı, 2014). More recently, DON was detected in 4 out of 60 wheat
(158–653 μg kg−1), 2 out of 25 pasta (52.2–61.0 μg kg−1) and only one
out of 25 rice samples (106.3 μg kg−1) collected from Turkey (Sahin,
2018, p. 79). However, this is first report on the occurrence of DON and
ZEA contamination in biscuits, and bread which is highly consumed
(about 320 g per day) in Turkey.
Wheat Maize
−1 −1
LOD (μg kg ) LOQ (μg kg ) LOD (μg kg−1) LOQ (μg kg−1)
21.70 72.30 14.08 46.90
1.12 3.70 1.06 3.50
3
O. Golge and B. Kabak
Table 2
The recovery, precision (intra-day repeatability and within-laboratory reproducibility) and expanded measurement uncertainty data in wheat and maize matrices.
Analyte Wheat
−1
Spiking level (μg kg ) Recovery (%) a
RSDr (%) RSDRb
DON 500 85.8 6.66 5.46
750 90.3 4.48 5.02
ZEA 50 105.1 5.08 4.91
100 103.3 3.61 2.30
a
RSDr: Intra-day repeatability.
b
RSDR: Within-laboratory reproducibility.
The contamination of cereal grains with Fusarium toxins is a
worldwide problem. The incidence of DON and/or ZEA in wheat and
other cereals has been reported in many countries, including Austria
(Berthiller et al., 2009), Brazil (Santos et al., 2013), China (Ji, Xu, Liu,
Yin, & Shi, 2014), Croatia (Pleadin et al., 2012), Czech Republic
(Polišenská, Sýkorová, Matĕ;jová, Chrpová, & Nedomová, 2008), Fin-
land (Nathanail et al., 2015), Hungary (Tima, Brückner, Mohácsi-
Farkas, & Kiskó, 2016), India (Mishra, Ansari, Dwivedi, Pandey, & Das,
2013), Italy (Alkadri et al., 2014), Korea (Ok et al., 2011), Morocco
(Ennouari, Sanchis, Marín, Rahuti, & Zinedine, 2013), Kenya
(Muthomi, Ndung'u, Gathumbi, Mutitu, & Wagacha, 2008), Poland
(Bryla et al., 2016), Serbia (Jajić, Jurić, Glamočić, & Abramović, 2008)
and Spain (Vidal, Marín, Ramos, Cano-Sancho, & Sanchis, 2013). It has
been shown that wheat samples were contaminated with DON with the
occurrence levels ranging from 3.5 to 100% and in concentrations up to
levels of 41 157 μg kg−1, depending on region climatic conditions,
seasonal variances, mould flora, agricultural practices, storage condi-
tions and the analytical method used in these researches. The incidence
of ZEA in wheat samples was 12.8% (10.1–3049 μg kg−1) in China (Ji
et al., 2014), 46.7% (1.9–234 μg kg−1) in Finland (Nathanail et al.,
2015), 17% (50–98 μg kg−1) in Hungary (Tima et al., 2016), 35%
(7–231 μg kg−1) in Italy (Alkadri et al., 2014), 13%
(327–1135 μg kg−1) in Romania (Stanciu, Juan, Miere, Loghin, &
Mañes, 2017), and 57% (1–96 μg kg−1) in Kenya (Muthomi et al.,
2008).
The studies showed that maize samples contained DON with the
incidence level of 100% in Austria (Berthiller et al., 2009), 72.5% in
Cameroon (Njobeh et al., 2010), 71% in Croatia (Pleadin et al., 2012),
86% in Hungary (Tima et al., 2016) and 32% in Serbia (Jajić et al.,
2008). According to these reports, the contamination of DON levels in
maize samples were from 10 to 3680 μg kg−1. In maize, the incidence of
ZEA was 87.5% and 41% in the samples from Croatia (Pleadin et al.,
2012), and Hungary (Tima et al., 2016), with concentration ranging
from 2 to 5110 μg kg−1, and from 54 to 565 μg kg−1, respectively.
The frequency of DON contamination in barley was 82.4%
(1.3–1180 μg kg−1) in Finland (Nathanail et al., 2015), 16%
(30–530 μg kg−1) in India (Mishra et al., 2013), 56%
(1.7–40.1 μg kg−1) in Korea (Ok et al., 2011) and 48%
(240–429 μg kg−1) in Hungary (Tima et al., 2016). Of the barley sam-
ples from Finland (n = 34), 5.9% were contaminated with ZEA, up to a
concentration of 17 μg kg−1 (Nathanail et al., 2015). DON was recorded
in rice with the incidences of 3.4–25.1%, and up to a level of
1355 μg kg−1 in Korea (Lee et al., 2011; Park, Choi, Hwang, & Kim,
2005).
Due to mycotoxins are highly stable compounds, it is not possible to
break down the entire toxins by heating or food processing, so it can be
found in heat-treated derived products. In contrast to our study, 94% of
17 wheat bread samples (13–350 μg kg−1) from Czech Republic
(Malachova et al., 2011), 28% of 75 samples (12.2–147 μg kg−1) from
Spain (González-Osnaya, Cortés, Soriano, Moltó, & Mañes, 2011), 79%
of 24 samples (7–270 μg kg−1) from Italy (Cirillo, Ritieni, Galvano, &
Cocchieri, 2003), 38% of 8 samples (37.5–78.1 μg kg−1) from Korea
Food Control 110 (2020) 106982
Maize
(%) Spiking level (μg kg−1) Recovery RSDr (%) RSDR (%) U ′ (%)
825 98.6 4.22 3.65 16.3
1750 98.4 2.27 2.17
175 102.7 1.57 6.48 21.0
350 97.4 7.75 5.48
(Ok et al., 2009) and 16.7% of 30 samples (140–1130 μg kg−1) from
Thailand (Poapolathep, Poapolathep, Klangkaew, Sugita-Konishi, &
Kumagai, 2008) gave positive results. With regard to pasta, the similar
DON incidence was reported in pasta consumed in Thailand
(Poapolathep et al., 2008), but levels were higher (170 and
350 μg kg−1) than found in this survey. In Italy, Cirillo et al. (2003)
detected DON in 8 out of 17 pasta samples (44%) at levels ranging from
9 to 77 μg kg−1, with a mean level of 19 μg kg−1. In another study
conducted in Spain, DON was found 47 out of 75 pasta samples
(62.7%), with concentrations ranging from 10.9 to 623 μg kg−1
(González-Osnaya et al., 2011).
In the group “cereals and bakery products”, maize and products
thereof are the most frequently notified issues (162 notifications) con-
cerned with mycotoxins in the Rapid Alert System for Food and Feed
(RASFF) portal, followed by rice (111 notifications) and wheat and
wheat-based products (53 notifications). Between 2002 and 2018, there
were 441 notifications in RASFF portal on mycotoxin hazard in cereals
and bakery products. AFs in cereals and derived products was the most
recurrent issue with 199 notifications, followed by OTA (92 notifica-
tions), FBs (91 notifications), DON (65 notifications) and ZEA (13 no-
tifications). There were 6 notifications on co-occurrence of DON and
ZEA in maize flour and maize-based products originating from Serbia,
Czech Republic, Belgium and Italy, with levels from 977 to
16 000 μg kg−1 for DON, and from 77 to 1000 μg kg−1 for ZEA.
In the RASFF portal, DON was the second most frequently notified
mycotoxins (22 notifications) after OTA in wheat and wheat-based
products. These notifications show that European countries such as
France, Czech Republic, Germany, Poland and Hungary were identified
19 times as the origin of the products with high levels of DON. For
pasta, there were only 7 RASFF notifications on mycotoxins, 4 of which
concerning DON, 2 of which concerning FBs and one of which con-
cerning OTA.
4. Conclusions
This study was designed to measure DON and ZEA contamination in
cereals and derived products commercialised in Turkey using HPLC
method. The sensitivity of the analytical method was suitable to meet
the limit of target mycotoxins established in the EU legislation and the
validation parameters meet the requirements of performance criteria
set in the Commission Regulation No 401/2006. DON was found in 26%
of wheat, 13.3% of maize, 20% of barley, 35% of paddy rice, 6% of
wheat flour, 10% of pasta and 20% of biscuits, but at levels well below
the respective EU ML. However, wheat bread and bulgur samples were
free from DON. For ZEA, 4% of wheat, 20% of maize, 55% of paddy rice
and 4% of wheat flour gave positive results, while barley, bulgur, wheat
bread, pasta and biscuit samples did not contain ZEA. Except for only
one paddy rice sample, all samples did not exceed respective EU ML for
ZEA. Further studies are needed to detect Fusarium toxins in cereals and
derived foods. It should be applied Codes of practices which describes
preventive measures established by Codex for the reduction biosynth-
esis both of free and masked forms of Fusarium toxins in cereals and
4
O. Golge and B. Kabak Food Control 110 (2020) 106982

MB (LB–UB): middle bound (lower bound–upper bound). LB: results below the LOD were replaced with 0, MB: results below the LOD were replaced with LOD/2, UB: results below the LOD were replaced with the
mycotoxin exposure.

P95 MB (LB–UB, μg Declaration of competing interest

1.12 (0–0.56)

1.12 (0–0.56)
No conflict of interest has been declared by the authors.
kg−1)

142.4

147.7
–f

–
–
–
–
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