Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
Research Article, Issue 2
Analytical Methods in Environmental Chemistry Journal
Journal home page: www.amecj.com/ir
AMECJ
Development of electrodeposited nanostructural poly
(o-aminophenol) coating as a solid phase microextraction
ber for determination of bisphenol A
Mohammad Saraji
a
, Bahman Farajmand*
,b
and Esmaeil Heydari Bafrouei
c
a
Department of Chemistry, Isfahan University of Technology, Isfahan, Iran.
b
Department of Chemistry, Faculty of Science, University of Zanjan, Zanjan, Iran.
C
Department of Chemistry, Vali-Asr University of Rafsanjan, Rafsanjan, Iran.
ABSTRACT
In this research nanostructural poly (o-aminophenol) was synthesized
by electropolymerization and used for solid phase microextraction
ber procedure (SPME). Thin lm of Poly (o-aminophenol) (4 µm
thickness) was shaped by sweep potential for 45 min on the surface
of stainless steel wire. Polymer was synthesized by potentiostat
procedure too. Prepared polymer by sweep potential procedure
showed nanostructures on the surface. Acetic anhydride was employed
for derivatization of bisphenol A (BPh-A) and analysis of acetylated
BPh-A was utilized by gas chromatography-ame ionization detector
(GC-FID). Affecting parameters on derivatization and extraction
such as amount of acetic anhydride, stirring rate, temperature, ionic
strength and extraction time were optimized. The limit of detection
(LOD) and relative standard divisions (RSDs%) were achieved 0.6
µgL
-1
and less than 6.8%, respectively under optimized conditions.
Finally proposed method was used for extraction of bisphenol A from
leaching of baby and drinking water bottles. Relative recovery was
achieved 98% for leaching from drinking bottle. In leaching from
plastic baby bottle, bisphenol A (BPh-A) was detected in the range
5–15 µg L
-1
.
Keywords:
Poly (o-aminophenol),
Nanostructure,
Bisphenol A,
Solid phase microextraction,
Gas chromatography-ame ionization
detector
ARTICLE INFO:
Received 10 Mar 2021
Revised form 28 Apr 2021
Accepted 25 May 2021
Available online 28 Jun 2021
*Corresponding Author: Bahman Farajmand
Email: farajmand@znu.ac.ir
https://doi.org/10.24200/amecj.v4.i02.142
------------------------
1. Introduction
Solid phase microextraction (SPME) is a simple,
solvent free and green sample preparation
technique which includes the employing of
a small amount of polymeric sorbent coated
on a thin ber for extraction [1]. Nowadays,
commercial SPME bers are available. The
important disadvantages of commercial SPME
bers are high cost, frangibility of the bers
and weakness of sorbents for extraction of polar
compounds. For domination of these drawbacks,
conductive polymers (CPs) such as polyaniline
(PANI) and polypyrole (PPy), coated on the
surface of metallic ber, are good choices [2]
but thermal instability of these CPs is a problem
when gas chromatography is applied for followed
analysis. Many solutions such as changing of
counter ion [3] or doping carbon nanotube [4] and
nanosilica [5] in the matrix of polymer, have been
suggested for modifying of thermal stability and
other properties of PANI and PPy. Application of
other new CPs with multi-functional groups can
be an alternative way for modifying of thermal
stability, selectivity and extraction efciency of
SPME bers.
35
Cadmium determination based on ISMP sensor Mohammad Saraji et al
Poly (o-aminophenol) (POAP) has been an
interesting polymer during three past decades.
Many of researches have been performed about
its synthesis, structure and application in sensor,
biosensor and corrosion protection [6]. The
POAP is formed by electrochemical oxidation of
o-aminophenol (o-AP) on the surface of different
electrode in aqueous solution. o-AP can be
polymerized electrochemically in alkaline, neutral
and acidic media. However, while a conducting
polymer lm is only produced in acidic media,
POAP prepared in neutral and alkaline media
leads to a nonconducting polymer lm so, the
polymer thickness of POAP synthesized in basic
and natural media is limited within 10–100 nm
due to a self-limiting growth [7]. The o-AP
is containing –OH and –NH
2
groups in ortho
position on a phenyl ring. Polymerization of the
o-AP can be performed by both groups therefore a
ladder structure could be formed which has better
thermal stability rather than PANI [8]. POAP
has been employed to build biosensors, because
it has been showed permselective properties
so the interference from different electroactive
species can be signicantly reduced during the
analysis of biological samples by utilizing a
biosensor based on POAP. Moreover, as both
hydroxyl and amino groups are involved in the
electropolymerization process of o-aminophenol,
large amounts of biological macromolecules
such as glucose oxidase [9,10] or horseradish
peroxidase [11] could be immobilized in poly(o-
aminophenol), which results in higher sensitivity
of the sensor as compared with sensors based on
other polymers. on the other hands the presence
of POAP as a sensing material can decrease the
oxidation overpotential of some molecules, so it
has shown the electrocatalytic behavior [12]. A
hybrid modied electrode was also prepared by
electropolymerization of o–AP in the presence
of sulfonated nickel phtalocyanine. The modied
electrode could electrocatalyze NO oxidation
and has been employed as NO sensor [13]. The
copolymer poly(aniline-co-o-aminophenol)
has been exhibited favorable properties to its
application in sensors, electrocatalysis, analytic
determinations and rechargeable batteries
[14,15]. The pH dependence of the electroactivity
of the copolymer is much better than that of
PANI. Poly(aniline-co-oaminophenol) has been
employed as sensor of catechol [16] and ascorbic
acid [17]. POAP has been applied as a molecular
imprinting polymer for sensor preparation. In this
regard, an electrochemical sensor for nicotine
based on the electropolymerization of o-PA as
monomer and nicotine as template was proposed
by Zhaoyang et al. [18]. Compared with nicotine
imprinting membranes, the POAP lm, was
homogeneous, had nanometric thickness and its
synthesis was easy. Other application of POAP
lm was reviewed by Tucerri [6].
Bisphenol A, (BPh-A), 2,2-bis(4-hydroxyphenyl)
propane, is one of the highest volume chemicals
in the world. It was applied for production of
polycarbonate with the second largest outlet being
epoxy resins [19]. A broad variety of food contact
materials stand out among their uses, mainly
derived from polycarbonates (infant feeding
bottles, storage containers, tableware, returnable
water, milk bottles and water pipes) and epoxy
resins (internal protective lining for food and
beverage cans, coating on metal lids for glass
jars and bottles and drinking water storage tanks)
[19]. The BPh-A has shown estrogenic activity
so it acts as an endocrine disruptor. Furthermore,
researches also has been indicated the potential
of BPh-A to disrupt thyroid hormone action [20],
to cause proliferation of human prostate cancer
cells [21] and to block testosterone synthesis [22]
at very low part-per-trillion doses So, there are
needs for introducing of new analytical procedures
particularly application of modern sample
preparation methods (such as microextraction
techniques) in order to have reliable tools for
control of human exposure to BPh-A. SPME with
commercial bers was utilized for extraction of
BPh-A frequently [23–27]. Molecularly imprinted
polymeric ber was employed for selective
extraction of BPh-A from complex matrix which
was shown by Tan et al. [28].
36
Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
The POAP, as a multi-functional group compound,
can be a remarkable sorbent for extraction of
different analytes so, in this paper, nanostructural
POAP coated on the stainless steel wire has been
prepared by electropolymerization under cyclic
voltametry and nally the polymeric coating was
used as a SPME ber for extraction of BPh-A from
aqueous matrix. Different effective parameters on
derivatization and extraction of BPh-A have been
evaluated and optimized and nally the method
has been applied for determination of BPh-A in
leaching from drinking and plastic baby bottle
that are made from polycarbonate.
2. Experimental
2.1. Materials
Bisphenol A was obtained from Sigma & Aldrich
(St. Louis, USA) and dissolved in methanol
to make stock solution at the concentration of
500 mg L
-1
. Intermediate standard solution was
prepared at concentration 10 mg L
-1
. More diluted
working solutions used in optimization studies
were prepared daily by diluting different amounts
of the intermediate standard solution with pure
water. All solutions were stored at 4
C prior to use.
HPLC grade methanol was purchased from Merck
(Darmstadt, Germany). Sodium dodecyl sulfate
(SDS), sulfuric acid, sodium chloride, sodium
sulfate and o-aminophenol were purchased from
Merck (Darmstadt, Germany). Sodium carbonate
and acetic anhydride for derivatization of BPH-A
was obtained from Merck too. Pure water was
prepared by OES (Overseas Equipment &
Services) water purication system (OK, USA).
The surgical grade stainless steel plunger of
a disposable spinal needle (27G, Bartar Co.,
Tehran, Iran) was used as the substrate of the
SPME bers.
2.2. Instrumentation
The SPME device was purchased from Supelco
(Bellefonte, PA, USA) and used for SPME
experiments with commercial bers (85 µm PA
and 65 µm PDMS/DVB). A homemade SPME
holder was assembled and used to perform
extraction with the bers produced in the
present work. A piece of stainless steel wire
(3 cm) was mounted into the SPME device
and used as a working electrode to make the
SPME ber. Electrochemical polymerization
was carried out with a potentiastat/galvanostat
AutoLab (Echo Chemie, Netherlands). A SP-
3420A gas chromatograph equipped with a split/
splitless injector and a ame ionization detector
(BFRL, Beijing, China) was employed for all
experiments. The injector was equipped with a
low-volume insert designed for the analysis by
SPME (Restek, Bellefonte, PA, USA). Nitrogen
(99.999%) was used as carrier and make-up
gas. The carrier and make-up gas ow rate was
set at 1.7 and 30 mL min
−1
, respectively. The
chromatographic separation was performed using
a DB-35ms, 10 m×0.25 mm, fused silica capillary
column with a 0.15 µm stationary phase thickness
(Supelco, Bellefonte, PA, USA). The injector
and detector temperatures were set at 260 and
280
C, respectively. The column temperature
was initially maintained at 100
C for 1 min;
subsequently, the temperature was increased to
250
C (at a rate of 30
C min
−1
) and held for 10
min. Surface characteristic studies of the poly
(o-aminophenol) coating was performed using
eld emission-scanning electron microscopy
(FE-SEM) (Hitachi, S-4160, Japan). Chemical
bonding characterization of the coating was
investigated using Fourier transform infrared
spectroscopy (FT-IR-350, Jasco Co., Tokyo,
Japan). Thermogravimetric analysis (TGA) was
performed using a Rheometric Scientic TGA
1500 instrument.
2.3. Preparation of SPME coating
Poly(o-aminophenol) lm was prepared according
to work of Kunimura et al [29] with some
modication. Polymerization was performed
with a potential-sweep electrolysis by using a
standard three-electrode cell. Stainless steel wire
(o.d. 0.2 mm) and platinum electrode were used
as working and counter electrodes. A length of 1
cm from the end part of stainless steel wire was
37
Cadmium determination based on ISMP sensor Mohammad Saraji et al
immersed into the polymerization solution. The
electrode potential was cycled between 0 and 1.3
V versus an Ag/AgCl electrode at 50 mV s
-l
in a
0.5 M Na
2
S0
4
solution (pH 1.0) containing 100
mM o-aminophenol and 0.05 mM SDS (as the
counter ion and catalyst). Solution was stirred
magnetically by a 1 cm stir bar at 800 rpm. For
the comparison purpose, polymer was synthesis
at a constant potential of 1.3 V for 45 min too. To
make the coating adhere rmly to the surface of
the wire, the wire surface was rst roughened by
a smooth sand paper and then washed in methanol
while sonicating. After polymerization, prepared
ber was thoroughly rinsed with distillated water
and thermally conditioned before use. Thermal
conditioning of the bers was carried out by
heating at 150
C for 20 min, then at 200
C for 20
min, and nally at 290
C for 20 h in a GC injector
port under a nitrogen atmosphere.
2.4. Derivatization and SPME procedure
A 3.0 mL standard solution of BPH-A containing
0.05 mol L
-1
of sodium carbonate was transferred
into a 7-mL glass vial from Supelco (14 mm
i.d.). A 13 mm×3 mm Teon coated stir bar
was used in the vial for stirring the solution.
For derivatization step, amount of 25 µL acetic
anhydride was added to the vial. The vial was
caped and reaction was performed for 5 min at 300
rpm and room temperature. After the reaction, 0.6
g of sodium chloride was added to the solution
and magnetically stirred until dissolving. For
extraction step, the SPME ber was immersed
into the sample solution under optimum stirring
rate (600 rpm) at room temperature. After 30
min, the ber was retracted into the needle and
immediately introduced into the GC injection
port (260
C). Injection was made in splitless
mode and desorption time obtained at 3 min.
3. Results and discussion
3.1. Characterization of POAP coating
The morphological structures of POAP coating
were investigated with FE-SEM and have been
shown in Figure 1. POAP coating prepared by
sweep potential showed granular structures
which were contained the large number of
nanoparticles (o.d. 50 nm or smaller) attached
to each other (Fig. 1a and b). However, in some
places, nanoparticles were placed beside each
other without any granular structure (Fig. 1d).
The thickness of the coating was obtained about
4 µm (Fig. 1c). It seems low conductivity of
polymer causes the thickness does not increase in
the period of electropolymerization [29]. Figure
1e and f demonstrate surface morphology of
POAP prepared by constant potential. As can be
seen, polymer lm is uniform and at and there
is no granular structure. Application of the ber
prepared by constant potential shows 4 times
weaker result than the one prepared by sweep
potential. It seems the higher surface area of the
polymer lm prepared by sweep potential plays
important role in extraction of analyte.
For gas chromatography applications, SPME
bers must be have efcient thermal stability.
The TGA curve of the POAP coating under argon
atmosphere at a heating rate of 10
C min
−1
has
been shown in Figure 2a. This lm was found to
start a slow loss of weight around 300
C. The
weight loss was at most 4% at this temperature
which could be attributed to the evaporation of
water moisture trapped in the pores of the lm.
So the present SPME ber coating is stable at
temperatures below 300
C due to ladder chemical
structure [29]. Then the ber is suitable for gas
chromatographic analysis.
Investigation of infrared spectroscopy of POAP
was carried out by many researchers and more
chemical structures have been proposed. o-AP
has two functional groups which contains –OH
and –NH
2
sites. Polymerization of o-AP can be
performed by both sites. Due to spectroscopic
measurements, different structures have been
proposed for POAP. Besides a completely ring-
closed or ladder structure with phenoxazine
units [8,30–32], other two structures, a partially
ring opened and another partially hydrolyzed,
have been considered for POAP. In-situ
Raman spectroscopy measurements propose
38
Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
that the POAP medium contains alternating
oxidized (quinonoid) and reduced (N-phenyl-
p-phenylenediamine) repeating units [33,34].
Zhang et al. introduced 1,4-substituted molecular
structure for POAP [33,34] allows explaining the
interaction of the polymer with metal ions. The
cation capturing process by POAP was certied
to simultaneous presence of -OH and –NH
2
groups of the polymeric backbone, in which the
lone-pair electrons are available to form metal
complex. IR studies have been indicated that the
POAP lm-growing process in alkaline media
involves the deprotonation of the aminophenol
molecule, which is probably chemisorbed at
the metal surface, followed by oxidation and
electropolymerization reactions. In this whole
process, the polymerization affects the –OH
group by the formation of C–O–C bond while the
–NH
2
groups are preserved [35].
In this study Fourier transform infrared
spectroscopy (FT-IR) was used to investigate the
functional groups of the polymer. Spectrum has
been revealed in Figure 2b. Broad peak between
3000 and 4000 cm
-1
assigned to the symmetric
stretching of NH and OH in aromatic system.
Strong peaks at 1582 and 1379 cm
-1
are belonging
to C-N stretching vibrations for quinoide structure
or combination band for protonated aromatic
amine [36]. Strong peak at 1460 cm
-1
can be
assigned for NH scissoring vibrations. Weak
peak at 1037 cm
-1
is belonging to C-C stretching
vibrations in benzene ring [36]. Consequently,
a blend of structures could be considered for
POAP lm. A weak peak at 2926 cm
-1
assigned to
stretching of CH in aliphatic system which can be
considered for dodecyl sulfate counter ion. SDS
plays two roles for preparation of POAP. At rst it
acts as a catalyst and oxidation potential of o-AP
was shifted to less positive potentials (almost
0.075V) and the oxidation current increased,
as compared with the process in the absence of
SDS. The rate of polymerization also increased
considerably in the presence of SDS [37] on the
other hands dodecyl sulfate has been used as a
frequent counter ion in conductive polymer
preparation that used for microextraction process
because it increases thermal stability of polymeric
lm [38].
Fig. 1. FE-SEM images from POAP coated on the surface of stainless steel wire at (a, b, c & d) cyclic potential
between 0 and 1.3 V with 50 mV/s rate; (e & f) constant potential at 1.3 V.
39
Cadmium determination based on ISMP sensor Mohammad Saraji et al
3.2. Optimization of conditions
For evaluation of POAP lm as a solid phase
microextraction ber, effects of various
parameters that can probably inuence the
performance of the derivatization and extraction
of BPH-A, including amounts of acetic anhydride
and sodium carbonat, salt concentration, stirring
rate, extraction time and temperature were
investigated. All experiments were performed
three times.
3.2.1.Optimization of derivatization conditions
Derivatization can reduce the polarity of some analytes
and can improve the extraction efciency and also
it leads to better peak shape, and higher sensitivity.
Acetic anhydride is a common derivatization reagent
that has been applied for blocking of hydroxyl group
of phenolic compounds frequently [23,39,40]. The
derivatization with acetic anhydride was performed
in situ. Consequently, the experimental variables
affecting to both the extraction and derivatization
processes were studied together. Derivatization
of bisphenol A with acetic anhydride performs in
basic condition. Sodium carbonate usually has been
used for adjustment of sample pH hence in this
research effect of different concentration of sodium
carbonate was investigated. Figure 3a show the
consequences. The concentrations of 0.05 and 0.1
Fig. 2. Thermal gravimetric analysis (a) and FT-IR spectra of POAP coating prepared by sweep potential.
40
Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
Fig. 3. (a) Effect of sodium carbonate concentration and (b) effect of acetic anhydride amount on the
derivatization efciency of bisphenol A (sample volume, 3 mL; concentration of analyte, 200 µg L
-1
; amount of
acetic anhydride (for (a)), 10 µL; amount of sodium carbonat (for (b)), 0.05 mol L
-1
; reaction time, 5 min; salt
addition, 0.1 g mL
-1
; stirring rate, 400 rpm; extraction time, 30 min).
mol L
-1
reveal maximum derivatization efciency,
Therefore, 0.05 mol L
-1
of sodium carbonate was
applied for adjustment of pH. Under optimized
pH, the amount of acetic anhydride was evaluated
for the best derivatization efciency. Effect of
different amount of acetic anhydride on extraction
efciency was summarized in Figure 3b. As can
be seen, concentration more than 0.75% (V/V) has
not signicant effect on derivatization efciency
therefore this concentration was selected as an
optimum point. Acetylation of phenolic compounds
usually is completed at a short time nonetheless in
this research the reaction time was studied too. The
results satisfy that the times more than 5 min have
not considerable effect on the reaction recovery (the
curve has not shown).
3.2.2.Optimization of extraction conditions
Effective parameters such as ion strength, stirring
rate, extraction temperature and time were
evaluated and optimized. The ion strength of the
sample solution was studied by spiking a series of
NaCl concentrations of 0–0.3 g L
-1
. The response
increases with the increase of ion strength; however,
the extraction efciency slightly decreases under
the high salt content (Fig. 4a). A salt level of
0.2 g mL
-1
of NaCl was used in the following
experiments. The ber is directly immersed in the
liquid samples, and partitions between the sample
matrix and the stationary phase were happened.
Agitation of the sample is often carried out with
a small stirring bar to decrease the time necessary
for equilibrium and to decrease the tension of the
static aqueous lm. The stirring bar is of dimension
10 mm × 3 mm. The effect of the stirring rate on
the responses was tested from 250 to 1000 rpm.
At a higher stirring rate of 600 rpm, a signicant
decrease in the area response was observed (Fig.
4b). Moreover, better result was obtained at a
relatively medium stirring rate than at the lower
and higher ones. Thus, a stirring rate of 600 rpm
was chosen for further experiments. Temperature
has kinetic and thermodynamic effects on
extraction recovery. On the other hands, solubility
of analyte in water increases at high temperature,
so, effect of temperature in the range of 10 to 45
C (Fig. 5a). Best results were achieved at 15
C
but for simplicity room temperature was applied as
an optimal temperature. The extraction time was
studied from 10 min to 60 min (Fig. 5b). The result
shows that the equilibrium time is reached until
40 min when a further increase of the extraction
time does not result in a signicant increase in the
detector response but for shortening the analysis
time, an extraction time of 30 min was established
in all the experiments.
41
Cadmium determination based on ISMP sensor Mohammad Saraji et al
3.3. Method validation
The linearity, the repeatability and the detection
limits of the proposed method were investigated.
The correlation coefcient (0.9981) indicated a good
linearity between 2 - 500 µg L
-1
. Under optimal
conditions, LOD was achieved 0.6 µg L
-1
. Relative
standard deviation for intra- and inter day were 4.0
and 6.1%, respectively. The amount of 6.8% was
attained for ber-to-ber relative standard deviation
too. On the other hands, extraction capability of the
POAP coated ber was compared with commercial
SPME bers. Poly acrylate (PA) and poly
dimethylsiloxane/divinylbenzen (PDMS/DVB)
commercial ber were chosen for this comparison.
Figure 6 shows the results. POAP coated ber
revealed better capacity for extraction of bisphenol
A. It seems the chemical composition and surface
congurations of coating are two effective factors
for this investigation. POAP has more chemical
functional groups compared to PA and PDMS/DVB
coating. On the other side, POAP nanostructure
morphology can help for more and fast extraction.
Fig. 4. (a) Effect of salt addition and (b) stirring rate on extraction of bisphenol A (sample volume, 3 mL; analyte
concentration, 200 µg L
-1
; 0.05 mol L
-1
sodium carbonate; amount of acetic anhydride, 25 µL; reaction time, 5 min;
stirring rate (for (a)), 400 rpm; salt addition (for (b)), 0.3 g mL
-1
; extraction time, 30 min at room temperature).
Fig. 5. (a) Effect of temperature and time on extraction of bisphenol A (sample volume, 3 mL; analyte concentration,
200 µg L
-1
; 0.05 mol L
-1
sodium carbonate; amount of acetic anhydride, 25 µL; reaction time, 5 min; stirring rate,
600 rpm; salt addition, 0.3 g mL
-1
; extraction time (for a), 30 min at room temperature (for b).
42
Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
3.4. Real sample analysis
To examine the feasibility of the method, new
SPME ber was applied for analysis of bisphenol A
released from milk and drinking water bottle. All the
leachate samples were collected from the containers
that had been lled with 50 mL of boiling hot water.
Bisphenol A was below the LOD for drinking
water bottle but was detected in the range 5–15 µg
L
-1
in leaching from plastic baby bottle. Relative
recovery was attained 98±3% for leaching from
drinking bottle. Relative recoveries were reported in
Table 1. Figure 7 shows the chromatograms from the
leaching of baby bottle with and without spiking of
bisphenol A. Releasing of bisphenol A from plastic
baby bottle was investigated in four time reusing and
the results were summarized in Figure 8. As can be
seen, bisphenol A exists in the consecutive leaching
but the amount of it reduces.
Fig. 6. Comparison of POAP coated SPME ber with PA & PDMS/DVB commercial ber (sample
volume, 3 mL; analyte concentration, 50 µg L
-1
; 0.05 mol L
-1
sodium carbonate; amount of acetic
anhydride, 25 µL; reaction time, 5 min; stirring rate, 600 rpm; salt addition, 0.3 g/mL; extraction
time, 30 min at room temperature).
Table 1. Relative recoveries of bisphenol A in different real samples (μg L
-1
)
Added Drinking water bottle Plastic baby bottle (1
st
leachate)
Found Relative
Recovery (%)
Found Relative
Recovery (%)
0.0 ND
*
- 15.1 -
10.0 9.7 97 25.4 103
20.0 20.6 103 35.3 101
50.0 51.0 102 64.1 98
100.0 94.1 94 109.1 94
* Not detected.
43
Cadmium determination based on ISMP sensor Mohammad Saraji et al
Fig. 7. GC-FID chromatograms after SPME of non-spiked (a) and spiked (b) leaching from plastic baby
bottle with 10 µg L
-1
of bisphenol A.
Fig. 8. Determined concentration of bisphenol A (BPH-A) in leaching from plastic
baby bottle after four time reusing.
44
Anal. Methods Environ. Chem. J. 4 (2) (2021) 34-46
Conclusions
This study shows application of nanostructural poly
(o-aminophenol) as a new SPME ber combined
with GC–FID is a precise method for reproducibly
analyzing trace bisphenol A from aqueous samples.
Better chromatographic shape and sensitivity were
obtained by derivatization of bisphenol A using
acetic anhydride. Different effective parameters
were studied and optimized. The gures of merit
belonged to the method were favorable. The
dynamic range was achieved in the ranges of 2 -
500 µg L
-1
. The limits of detection and RSD were
0.6 µg L
-1
and <6.8% respectively. The feasibility
of using the SPME–GC–FID system to measure the
amount of bisphenol A in leaching from plastic baby
and drinking water bottle was tested. Bisphenol A
was detected in the range 5–15 µg L
-1
.
5.Acknowledgment
The authors are grateful to the Research Council
of Isfahan University of Technology (IUT) and
the Center of Excellence for Sensor and Green
Chemistry for their support of this project.
6. References
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Namie, Recent developments and future trends
in solid phase microextraction techniques
towards green analytical chemistry, J.
Chromatogr. A, 1321 (2013) 1–13.
[2] M. Lashgari, Y. Yamini, An overview of the
most common lab-made coating materials
in solid phase microextraction, Talanta, 191
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