Food Analytical Methods (2020) 13:1799–1805

https://doi.org/10.1007/s12161-020-01788-2

A Novel Method for Chlorine and Sulfur Determination in Gluten-Free

and Gluten-Containing Edible Flours from Different Raw Materials
and Countries
Marcia F. Mesko 1 & Vanize C. Costa 1 & Jussiane S. Silva 2 & Priscila T. Scaglioni 1 & Angelica C. Frohlich 2 &
Fabio A. Duarte 2 & Erico M. M. Flores 2

Received: 7 January 2020 / Accepted: 31 May 2020 / Published online: 24 June 2020
# Springer Science+Business Media, LLC, part of Springer Nature 2020

Abstract
A novel and eco-friendly analytical method using microwave-induced combustion (MIC) and ion chromatography (IC) was
proposed for the determination of chlorine and sulfur in corn, potato, rice, and wheat edible flours from several countries (Austria,
Brazil, Belgium, Ecuador, Poland, and Turkey). Agreement with certified reference material (NIST 1568a, rice flour) was 97%
for Cl and 90% for S. The limits of quantification were 5.2 μg g−1 for Cl and 1.5 μg g−1 for S. The content of elements did not
vary significantly between wheat flours from different countries. The highest concentration of Cl and S was found in wheat flours
(Cl: 424 to 714 μg g−1; S: 1020 to 1477 μg g−1) when compared with corn (Cl: 330 to 408 μg g−1; S: 751 to 895 μg g−1), rice (Cl:
204 to 219 μg g−1; S: 1007 to 1041 μg g−1), and potato starch flours (Cl < 5.2 μg g−1; S: 8.44 to 11.2 μg g−1). It is important to
highlight that the proposed method presents low limits of detection, low relative standard deviations, and high sample throughput,
which indicates that it is an excellent alternative as a new analytical method that could be used for routine analysis of edible
flours.

Keywords Edible flour . Microwave-induced combustion . Sample preparation . Chlorine determination . Sulfur determination .
Ion chromatography

Introduction
Wheat is considered an important alimentary source and one
of the “big three” cereal crops, together with rice and corn
(FAO 2015; Shewry 2009). However, this cereal is usually
milled and converted to flour before consumption, which
may result in losses of nutrients from the whole grain and/or
contamination of the produced flour (Shewry 2009).
Moreover, some exogenous components may be used to im-
prove the breadmaking capacity of wheat flour, such as oxi-
dizing agents and enzymes (Joye et al. 2009). These additives
include chlorine- and sulfur-containing compounds and have
* Marcia F. Mesko
marcia.mesko@pq.cnpq.br
1 amino acids (proteinogenic and non-proteinogenic) and pep-
Centro de Ciências Químicas, Farmacêuticas e de Alimentos,
Universidade Federal de Pelotas, Capão do Leão, RS 96160-000,
Brazil
2
Departamento de Química, Universidade Federal de Santa Maria,
Santa Maria, RS 97105-900, Brazil
also been used in gluten-free flours, like those from corn,
potato, and rice, for simulating the viscoelastic properties of
gluten, as well as acceptability and shelf-life of these products
(Joye et al. 2009; Nimni et al. 2007; Shewry 2009). In this
sense, the presence of Cl and S in edible flours depends on
several factors such as the soil composition, plant genotype,
and the use of fertilizers and pesticides during the cultivation
of raw materials as well as of flour treatment agents used
during the processing (Joye et al. 2009; Nimni et al. 2007).
Although the essentiality and toxicity of all the halogens to
the organisms are still not well known, Cl is considered an
essential element (Mello et al. 2013; Serfor-Armah et al.
2002). This element, when present as chloride form, contributes
to the maintenance of the normal fluid balance inside and out-
side cells, as well as the balance of acids and bases in the body
(Serfor-Armah et al. 2002). Sulfur also plays important func-
tions in the human body, since it is one of the constituents of
tides involved in key cellular processes (Cornelis et al. 2005).
Thus, the determination of Cl and S in gluten-free or gluten-
containing flours is important considering that regulatory insti-
tutions have not established a limit for the total content of Cl
1800
and S in edible flours. It is important to mention that there are
maximum limits only for some substances containing Cl or S,
which are commonly used as flour treatment agents (Food and
Drug Regulations - C.R.C., c. 870. Government of Canada
2016). Despite the known variability in the composition of
edible flours due to the origin of raw material and the use of
additives, especially in gluten-free flours, there are few studies
in the literature regarding the non-metal determination in these
food matrices (Gois et al. 2015; Mesko et al. 2010; Olise et al.
2014; Pereira et al. 2014; Silva et al. 2017).
The determination of non-metals in flours has been per-
formed by direct analysis or by inductively coupled plasma
mass spectrometry (ICP-MS) (Gois et al. 2015; Mesko et al.
2010; Olise et al. 2014; Pereira et al. 2014; Silva et al. 2017).
The determination of non-metals in edible flours by direct
analysis was previously applied for Cl determination using
solid sampling and electrothermal vaporization (SS-ETV)
ICP-MS (Gois et al. 2015) and high-resolution continuum
source graphite furnace molecular absorption spectrometry
(HR-CS GF MAS) (Pereira et al. 2014), and for bromine
and potassium determination using the particle-induced X-
ray emission (PIXE) technique, which requires little or even
no sample preparation (Olise et al. 2014). These methods
show suitable performance for some samples/analytes and
avoid extensive sample preparation. However, the lack of
standards for calibration and the requirement of a very homo-
geneous sample can affect the precision and accuracy of the
results obtained by direct analysis (West et al. 2016). On the
other hand, a suitable sample preparation step is required prior
to the analysis by ICP-MS to avoid physical and spectral in-
terferences (Mesko et al. 2016).
Concerning the determination of Cl and S in organic ma-
trices, several analytical techniques have been used (Bu et al.
2003; Mello et al. 2013; Ozbek and Baysal 2017; Schnetger
and Muramatsu 1996). Among these techniques, the plasma-
based techniques and ion chromatography (IC) are extensively
used due to the suitable selectivity and sensitivity for non-
metal determination (Mello et al. 2013; Ozbek and Baysal
2017). However, high ionization potentials, low wavelength
emission lines, and spectral and non-spectral interferences
make the determination of non-metals by argon plasma-
based spectrometric techniques a difficult task, especially
when compared with the determination of metals.
Ion chromatography is an interesting alternative due to its
ease of operation and low instrumentation and operation costs
when compared with plasma-based techniques, such as ICP-
MS and inductively coupled plasma optical emission spec-
trometry (ICP OES) (Ozbek and Baysal 2017). However, both
of these techniques generally require a sample preparation
step to obtain solutions containing the analytes and preferen-
tially free from the sample matrix (Mello et al. 2013). For this
purpose, considering the major organic composition of edible
flours and the unsuitability of wet digestion using
Food Anal. Methods (2020) 13:1799–1805
concentrated acids for the subsequent halogen determination,
such as Cl, combustion methods are considered the most suit-
able alternative (Flores 2014).
Microwave-induced combustion (MIC) has been used for
the digestion of several types of samples (such as animal feed,
human hair, crude oil, cereals, legumes, and egg powder) for
the subsequent determination of non-metals due to its high
efficiency for organic matrix digestion and capability to pro-
vide digests compatible with most of detection techniques
(ICP-MS and also IC) (Barin et al. 2014; Novo et al. 2018;
Mesko et al. 2019; Pereira et al. 2015; Rondan et al. 2019;
Toralles et al. 2017). MIC has been previously applied by our
research group for the digestion of edible flours and subse-
quent determination of Br and I by ICP-MS (Silva et al. 2017).
However, its suitability for the subsequent determination of Cl
and S in edible flours has not yet been evaluated. MIC has also
been considered a relatively fast digestion method that mini-
mizes the reagent consumption and contributes to the achieve-
ment of low limits of detection (LODs) (Barin et al. 2014).
Gluten-free edible flours could be used directly in food
production as a new raw material type in the future.
However, to achieve this goal, it is necessary to know the
proximate composition, mineral contents, and nutritional and
health-related values of these flours, and, until now, limited
information has been available on the mineral content, espe-
cially for Cl and S, from the different raw materials. Thus, this
study aimed to develop a method for the determination of Cl
and S in edible flours by IC after sample digestion by MIC.
Moreover, we also aimed to obtain information related to Cl
and S content in gluten-free and gluten-containing edible
flours from different raw materials from six countries.
Material and Methods
Instrumentation
The MIC method was carried out using a microwave sample
preparation system (Multiwave 3000, Anton Paar, Austria)
equipped with up to eight closed quartz vessels with an inter-
nal volume of 80 mL and maximum temperature and pressure
of 280 °C and 80 bar, respectively. A commercial quartz hold-
er (Anton Paar) was used in the MIC procedure.
An analytical balance (AY 220, Shimadzu, Japan) with a
maximum capacity and resolution of 220 and 0.0001 g, re-
spectively, was used for sample weighing. Flour pellets of
13 mm diameter were prepared (3 ton for 1 min) before di-
gestion by MIC using a hydraulic press (Manual Hydraulic
Press 15 Ton, Specac, UK).
Ultrapure water (18.2 MΩ cm) was obtained using a puri-
fication system (Milli-Q system, Millipore, USA). Moreover,
an ultrasonic bath (Elmasonic X-tra 50 H, Elma, Germany)
and a class 100 laminar flow bench (CSLH-12, Veco, Brazil)
Food Anal. Methods (2020) 13:1799–1805
were used for the decontamination of some materials used
during the sample preparation.
For the determination of Cl (as chloride) and S (as sulfate),
an ion chromatographic system (850 Professional IC,
Metrohm, Switzerland) was used. This system was equipped
with an anion-exchange column (Metrosep A Supp 5, polyvi-
nyl alcohol with quaternary ammonium groups, 150 × 4 mm
i.d.), a guard column (Metrosep A Supp 4/5 Guard), an anion
self-regeneration suppressor, and a conductivity detector. A
sample loop of 100 μL was used and the mobile phase flow
rate was set at 0.7 mL min−1.
For comparison of results, the determination of Cl and
S was performed using an inductively coupled plasma
optical emission spectrometer (Optima 4300 DV,
PerkinElmer, USA), equipped with a GemCone® nebuliz-
er and a cyclonic spray chamber. The carbon content in
digests was also determined by ICP OES. The plasma
radiofrequency power was set at 1400 W for C determi-
nation and at 1600 W for the determination of Cl and S.
Argon 99.998% (White Martins, Brazil) was used for
plasma generation, and as auxiliary and nebulizer gases
(14.0, 1.0, and 0.85 L min−1, respectively). Carbon, Cl,
and S were determined at 193.091, 134.724, and 180.731
nm, respectively.
Reagents
All solutions and dilutions were prepared using ultrapure wa-
ter and all reagents used in this study were of analytical grade.
The absorbing solutions of ammonium hydroxide or am-
monium carbonate were prepared from 28% NH4OH solution
(Merck, Germany) and (NH4)2CO3 salt (Merck), respectively.
A 6 mol L−1 NH4NO3 solution was used as combustion ignit-
er, and it was prepared by dissolving the solid reagent (Merck)
in water.
Small discs of filter paper (15 mm diameter, 15.3 ± 0.3 mg)
with low ash content (Black Ribbon Ashless, Schleicher and
Schuell GmbH, Germany) were used as combustion aid.
Before using, paper discs were decontaminated with ethanol
(Vetec, Brazil) in an ultrasonic bath (2 steps of 20 min each),
rinsed with water and dried in a class 100 laminar flow bench.
Oxygen (99.6%, White Martins) was used for the pressuriza-
tion of quartz vessels for the MIC method.
The cleaning of vessels and holders was performed in the
same microwave oven used for sample digestion, but using 6
mL of 14.4 mol L−1 HNO3 (Vetec) at 1000 W for 10 min and
0 W for 20 min (cooling step). Further, a second cleaning step
was performed using 6 mL of water instead of 14.4 mol L−1
HNO3.
Stock standard solutions containing 10,000 mg L−1 of
−
Cl or SO42− were prepared by dissolution of sodium
chloride (Merck) or sodium sulfate (Merck) in water.
Standard solutions used for the determination Cl and S
1801
in edible flours by IC and ICP OES were prepared by
dilution of stock solutions in water, NH4OH (10 mmol
L−1) or (NH4)2CO3 (10 mmol L−1). These solutions were
the same as those used as absorbing solution for the MIC
procedure. Recovery tests were performed using a stan-
dard solution containing 3000 mg L−1 Cl− and 10,000 mg
L−1 SO42−, which was also prepared by the dissolution of
salts in water.
The mobile phase solution for IC measurements was com-
posed of 3.2 mmol L−1 sodium carbonate and 1.0 mmol L−1
sodium bicarbonate solution, and it was prepared by dissolu-
tion of Na2CO3 and NaHCO3 in water.
Citric acid (Merck) was dissolved in water and the obtained
solution (1000 mg L−1 C) was used to prepare standard solu-
tions (10 to 500 mg L−1 in 0.7 mol L−1 HNO3) for the deter-
mination of C by ICP OES. Yttrium solution (1000 mg L−1,
Fluka, USA) was used as an internal standard and added to all
samples and standard solutions at a final concentration of
1 mg L−1. Argon was also used (0.1 L min−1 for 2 min) for
the removal of volatile carbon compounds in digests before C
determination.
Samples and Accuracy Evaluation
Fifteen samples of edible flours were purchased from dif-
ferent countries (Austria, Belgium, Brazil, Ecuador,
Poland, and Turkey). These samples were labeled as S1
to S15 (values informed by the manufacturer for carbohy-
drate content ranged from 64 to 83%, protein from 0.1 to
12%, fat from 0 to 3%, and dietary fiber from 1 to 12%).
Samples included wheat flour (S1 to S6), whole wheat
flour (S7 to S9), corn flour (S10 and S11), potato starch
flour (S12 and S13), and rice flour (S14 and S15). Sample
S1 was arbitrarily selected for the method development
and other samples were analyzed using the optimized con-
ditions. Before analysis, samples were dried at 105 °C for
2 h using a conventional oven.
The accuracy of the method was determined by the
analysis of a CRM (NIST 1568a, rice flour) from the
National Institute of Standards and Technology (NIST,
USA) and by analyte recovery tests. The limit of quanti-
fication (LOQ) of the proposed method was estimated
according to that described by the International Union of
Pure and Applied Chemistry (IUPAC) (Currie 1995).
Thus, the LOQ was calculated by the sum of mean and
standard deviation (SD) of ten measurements of blank
solutions obtained after MIC in the absence of the sample.
Before, the SD obtained for ten measurements of blank
was multiplied by a factor (IUPAC default value is 10).
Moreover, to obtain the LOQ in “μg g−1,” the final vol-
ume (25 mL) of digest and the sample mass were also
considered. All the statistical evaluations were carried
out using GraphPad InStat software (GraphPad InStat
1802 Food Anal. Methods (2020) 13:1799–1805

Software Inc., Version 3.06, USA, 2003) with a confi-

dence level of 95%.

Sample Digestion by MIC and Cl and S Determination

by IC—Method Optimization

Edible flour samples (1000 mg) were pressed to obtain the

pellets, which were placed together with a small disc of filter
paper on a quartz holder. Ammonium nitrate solution (50 μL,
6 mol L−1) was added to the paper and the quartz holder was
introduced into the quartz vessel containing 6 mL of absorb-
ing solution. The evaluated absorbing solutions were water
and solutions of NH4OH and (NH4)2CO3 (10, 25, or 50 mmol
L−1). Vessels were closed, positioned in the rotor, and pres-
surized with 20 bar of oxygen. The rotor with vessels was Fig. 1 Chlorine (white bars) and S (gray bars) concentration after
digestion of edible flour (sample S1) by MIC using water, 10, 25, or
placed inside the microwave oven and the irradiation program 50 mmol L−1 NH4OH or 10, 25, or 50 mmol L−1 (NH4)2CO3 as the
(1400 W for 5 min and 0 W for 20 min) was started. After absorbing solution. Determination by IC (error bars represent the
combustion, digests were diluted with water up to 25 mL for standard deviation, n = 3)
further determination of Cl and S by IC.
consumption and waste generation and contributes to simplify the
procedure. Besides, relative standard deviations (RSDs) lower
Results and Discussion than 6% were obtained using all the solutions (concentration level
of 637 ± 20 μg g−1 for Cl and 1271 ± 64 μg g−1 for S). Thus,
Digestion of Edible Flours by MIC and Cl and S water was selected as the absorbing solution for the subsequent
Determination by IC—Method Optimization studies, once that it also contributes to the compatibility of the
digests with the IC technique. Chromatograms for standard solu-
The sample mass (1000 mg) used in the present study was tion containing 0.75 mg L−1 of Cl− and 7.5 mg L−1 of SO42− and
based on previous work published by our research group that the sample S1 prepared by the MIC method using the optimized
aimed the determination of Br and I in edible flours (Silva condition are presented in Fig. 2. The total time of chromato-
et al. 2017). The pressure achieved during the combustion of graphic run for sequential determination of both elements was
1000 mg of edible flour was lower than 40 bar, which was 30 min using suppressed conductivity detection. During the de-
about 50% of the operational pressure limit (80 bar). Low termination of Cl− and SO42− by IC, dilution factors up to 30
carbon concentration in digests (below 20 mg L−1) was ob- times were performed when necessary, depending on the analyte
tained after MIC, indicating that 1000 mg of edible flours was concentration in the digests.
efficiently and safely digested.
To select the most suitable solution for IC analysis and to
absorb Cl and S after sample combustion, water and solutions
of NH4OH and (NH4)2CO3 (10, 25, and 50 mmol L−1) were
evaluated. These solutions were selected according to previ-
ous works that aimed the determination of Cl and S in other
matrices (Pereira et al. 2009, 2015), as well as because the use
of acid solutions may cause analyte losses by volatilization,
especially for Cl, and generally they are not compatible with
chromatographic analysis (Flores 2014). The results for Cl
and S determination by IC in different absorbing solutions
are shown in Fig. 1.
As can be seen in Fig. 1, the results for Cl and S did not present
statistical differences (Tukey test, 95% of confidence level) after
digestion of sample S1 by MIC, indicating that all of the evalu-
ated solutions were suitable for the absorption of the analyte. It is
Fig. 2 Chromatograms obtained for chloride (0.75 mg L−1) and sulfate
important to point out that even when using water as the absorb- (7.5 mg L−1) standard solution (▬) and for wheat edible flour digests
ing solution the results for Cl and S were satisfactory, which is an obtained by the MIC method using water as the absorbing solution (▬)
advantage over the other solutions because it minimizes reagent (dilution factor of 30 times)
Food Anal. Methods (2020) 13:1799–1805 1803

In order to determine the recoveries of Cl and S after MIC important for the determination of Cl and S in samples of potato
method, 100 μL of a reference solution (containing 3000 mg starch flour (as can be seen in Table 1), are related mainly to the
L−1 Cl− and 10,000 mg L−1 SO42−) was added to the pellet of possibility of digesting a high sample mass (1000 mg) and the
sample S1 (1000 mg) before digestion by MIC using water as compatibility of the digests with the determination technique, as
absorbing solution. The recoveries for Cl and S were 103 ± 6 well as the low blank values for both analytes. In addition, the
and 108 ± 4% (n = 3), respectively. Accuracy of the method proposed method presents relatively high throughput (up to 16
was determined by the analysis of CRM NIST 1568a (rice samples can be digested per hour, and both analytes can be
flour) and by comparison of the results obtained by IC with determined in less than 30 min), allows low reagents consump-
those determined by ICP OES. As can be seen in Table 1, the tion, and minimizes the generation of laboratory wastes.
results for the CRM were in agreement (97% for Cl and 90%
for S) with informed and certified values, respectively. In ad-
dition, the results for the determination of Cl (592 ± 30 μg g−1) Determination of Cl and S Gluten-Free and Gluten-
and S (1250 ± 38 μg g−1) by ICP OES for sample S1 did not Containing Edible Flour
show statistical difference (Student’s t test, 95% of confidence
level) with those obtained by IC (637 ± 20 μg g−1 for Cl and Taking into account the suitability of MIC for the digestion of
1271 ± 64 μg g−1 for S). Therefore, the proposed method has edible flours and subsequent determination of Cl and S by IC,
suitable accuracy for the determination of Cl and S in edible the proposed method was applied for the digestion of edible
flours by IC, making it a promising method that employs high flours from different raw materials (corn, potato, rice, and
sample mass and water as the absorbing solution in the diges- wheat) and countries (Austria, Belgium, Brazil, Ecuador,
tion by MIC, which is suitable for IC analysis. Poland, and Turkey). These experiments were performed
It is important to mention that, using the optimized conditions, using optimized conditions (1000 mg of sample and water
the LOQs for Cl and S were 5.2 and 1.5 μg g−1, respectively. The as the absorbing solution). The results are shown in Table 1.
LOQ for Cl was comparable with those obtained in other studies The concentration of S was higher than the Cl concentra-
which used techniques based on direct sample analysis for Cl tions in all samples. Probably, this behavior is related to the
determination in edible flours by SS-ETV-ICP-MS (Gois et al. presence of proteins containing interchain disulfide bonds in
2015) and by HR-CS GF MAS (Pereira et al. 2014). The low this type of matrix (Shewry 2009). It is important to emphasize
LOQ values obtained for the proposed method, which were that the results for S are in agreement with those reported in the
literature, since gluten proteins, which contain S in their com-
position, are located in the endosperm tissue (Shewry 2009).
Table 1 Concentration of Cl and S in edible flours after MIC using
water as absorbing solution, 1000 mg of sample, and further The rice flours presented S concentration (1007 to 1041 μg
determination by IC (mean ± standard deviation, n = 3, μg g−1) g−1) relatively similar to that of the analyzed wheat flours
(1020 to 1477 μg g−1). This behavior may be related to the
Sample (raw material, country) Cl S
presence of glutelin, which is the main protein of rice, consti-
S1 (wheat flour, Brazil) 637 ± 20 1271 ± 64 tuting at least 80% of the total protein in the endosperm
S2 (wheat flour, Belgium) 614 ± 23 1309 ± 32 (Cagampang et al. 1966). On the other hand, the concentration
S3 (wheat flour, Austria) 714 ± 56 1403 ± 109 of Cl and S in other types of edible flours (samples S10 to
S4 (wheat flour, Ecuador) 604 ± 16 1477 ± 31 S15) studied was lower than those obtained from wheat flours
S5 (wheat flour, Poland) 527 ± 14 1020 ± 41 (S1 to S9), especially in potato starch flours (the concentration
S6 (wheat flour, Turkey) 627 ± 32 1260 ± 61 was below 5.2 μg g−1 for Cl and from 8.44 to 11.2 μg g−1 for
S7 (whole wheat flour, Brazil) 609 ± 19 1322 ± 64
S). These types of flours have lower protein content (0.1 to
S8 (whole wheat flour, Brazil) 479 ± 13 1224 ± 55
7.4%) than wheat flours (10 to 12%), which may be an im-
S9 (whole wheat flour, Brazil) 424 ± 17 1405 ± 106
portant source of S. In addition, the amino acid composition of
potatoes is minimally represented by sulfur containing amino
S10 (corn flour, Brazil) 408 ± 13 895 ± 43
acids (methionine and cysteine), which represent 1 to 3% of
S11 (corn flour, Brazil) 330 ± 11 751 ± 51
the total protein content in this tuber (Jadhav and Kadam
S12 (potato starch flour, Poland) < 5.2** 11.2 ± 0.8
1998). Besides that, the traditional potato flour or starch ap-
S13 (potato starch flour, Brazil) < 5.2** 8.44 ± 0.68
plied in potato stable products is usually obtained through a
S14 (rice flour, Brazil) 219 ± 11 1041 ± 51
series of processing steps, which brought damage to nutrition-
S15 (rice flour, Brazil) 204 ± 10 1007 ± 36
al components such as protein and dietary fiber (Zhang et al.
NIST 1568a (rice flour)* 292 ± 8 1075 ± 42
2017). In addition, the protein and fat contents in potato
*Informed value for Cl of 300 μg g−1 ; certified value for S of 1200 ± 2 μg starches are usually negligible in this type of flour, whereas
g−1 high levels of protein and some fat are present in wheat flour
**LOQ (Zaidul et al. 2008). Thus, it can be inferred that the lower
1804
values found for Cl and S concentrations in potato starch
flours were also consequences of this raw material processing.
Regarding the concentration of Cl in edible flours, it is also
important to mention that results are in agreement with a study
reported in the literature, once wheat, corn, and rice flours pre-
sented the highest, intermediate, and lowest concentrations of Cl,
respectively, when compared with each other (Hager et al. 2012).
Conclusions
The obtained results indicate that the variations in the concen-
tration of Cl and S may be related mainly to the type of raw
material used to produce the flour. Moreover, the results
showed that the proposed method using MIC and IC was suit-
able for the evaluation of Cl and S concentration in gluten-free
and gluten-containing edible flours. Thus, the MIC method was
efficient to digest high sample mass (up to 1000 mg) indepen-
dently of the edible flour composition. In addition, the MIC
provided solutions compatible with ion chromatography anal-
ysis, avoiding the occurrence of interferences and eliminating
additional dilution steps. By using the proposed method, results
with good accuracy and precision, as well as low LOQs and
blank values, were obtained. All these characteristics allow the
determination of Cl and S in most of the edible flours analyzed,
even when the analytes are present in low concentration.
Funding Information This study was financially supported by the
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - Brazil
(CAPES) - Finance Code 001, as well as Conselho Nacional de
Desenvolvimento Científico e Tecnológico (CNPq - Brazil), grant num-
ber 409357/2016-2; Instituto Nacional de Ciência e Tecnologia de
Bioanalítica (INCTBio CNPq - Brazil), grant number 465389/2014-7;
and Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul
(FAPERGS - Brazil), grant numbers 16/2551-0000561-8 and 19/2551-
0001306-0.
Compliance with Ethical Standards
Conflict of Interest Marcia F. Mesko declares that she has no conflict of
interest. Vanize C. Costa declares that she has no conflict of interest.
Jussiane S. Silva declares that she has no conflict of interest. Priscila
Tessmer Scaglioni declares that she has no conflict of interest. Angelica
C. Frohlich declares that she has no conflict of interest. Fabio A. Duarte
declares that he has no conflict of interest. Erico M. M. Flores declares
that he has no conflict of interest.
Ethical Approval This article does not contain any studies with human
participants or animals performed by any of the authors.
Informed Consent Not applicable.
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