Science of the Total Environment xxx (xxxx) xxx

Contents lists available at ScienceDirect

Science of the Total Environment

journal homepage: www.elsevier.com/locate/scitotenv

Occurrence, fate and environmental risk of anionic surfactants,

bisphenol A, perfluorinated compounds and personal care products in
sludge stabilization treatments
Concepción Abril, Juan Luis Santos ⇑, Julia Martín, Irene Aparicio, Esteban Alonso
Departamento de Química Analítica, Escuela Politécnica Superior, Universidad de Sevilla, C/ Virgen de África, 7, E–41011 Sevilla, Spain

h i g h l i g h t s g r a p h i c a l a b s t r a c t

The highest concentrations

corresponded to surfactants, biocides
and UV filters.

Anaerobic stabilization was the most
effective treatment for the removal of
EDCs.

Biocides and BPA were not removed
in any of the studied sludge
treatments.

After sludge application onto soils,
only TCS involved environmental
risks.

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

Article history: In this work, twenty-three endocrine disrupting compounds have been monitored in sludge from differ-
Received 7 August 2019 ent stages of four sludge stabilization treatments (anaerobic digestion, aerobic digestion, composting and
Received in revised form 26 September anaerobic stabilization ponds). Their occurrence and fate in sludge stabilization plants and their potential
2019
environmental risk in treated sludge and in treated sludge-amended soils have been evaluated.
Accepted 16 October 2019
Available online xxxx
Monitored compounds were six perfluoroalkyl compounds (PFC), four anionic surfactants (sodium alkyl-
sulfates), a plasticiser (bisphenol A (BPA)), four preservatives (parabens), six UV-filters (benzophenones)
Editor: Paola Verlicchi and two biocides (triclosan and triclocarban). Only two of the UV-filters were not detected in any of the
141 analysed samples. Anionic surfactants (mean concentrations up to 1673 ng/g dry matter (dm) for the
Keywords: sum of surfactants) were the compounds at the highest concentration levels followed by biocides (up to
Endocrine disrupting compounds 512 ng/g dm) and UV-filters (up to 662 ng/g dm). The concentrations of anionic surfactants, preservatives
Sludge stabilization technologies and UV-filters decreased 78, 25 and 80%, respectively, after anaerobic digestion. The concentration of per-
Sorption fluorinated carboxylic acids only decreased after composting (80% reduction) whereas biocides and BPA
Biodegradation were not affected by any of the studied treatments. Environmental risks (risk quotients > 1) were
Sludge environmental risks obtained for all compounds, except for triclocarban and sodium octadecylsulfate, in treated sludge. In
Sludge-amended soils
treated sludge-amended soils, risk quotients were lower than 1 for all compounds except for triclosan.
Ó 2019 Elsevier B.V. All rights reserved.

1. Introduction

⇑ Corresponding author at: Department of Analytical Chemistry, University of Currently, the most common sludge stabilization treatments are
Seville, C/ Virgen de África, 7, 41011 Seville, Spain. anaerobic digestion (applied in anaerobic treatment plants (AnTP)),
E-mail address: jlsantos@us.es (J.L. Santos). aerobic digestion (applied in aerobic treatment plants (AeTP)),

https://doi.org/10.1016/j.scitotenv.2019.135048
0048-9697/Ó 2019 Elsevier B.V. All rights reserved.

Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
2 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx
composting (applied in composting plants (CP)) and, in small cities,
anaerobic digestion in anaerobic stabilization ponds (AnSP) (Anjum
et al., 2016, Martín et al., 2015). In Europe, 39% out of the 10.13 mil-
lion tons dry matter (d.m.) annually generated of treated sludge are
estimated to be spread on agricultural lands as fertilizer (Milieu
et al., 2008). In some countries, sludge application onto soils is even
higher than 60% (France: 70%; United Kingdom: 68%; Ireland: 63%
(Milieu et al., 2008); Spain: 76% (MMARM, 2010)). However, sludge
application onto soils can involve negative effects such as odours
(Rincón et al., 2019) and contamination with pollutants sorbed into
sludge from wastewater that can enter into the food chain (Zhang
et al., 2015; Aparicio et al., 2018; Urra et al., 2019). To the date,
the pollutants usually monitored in sludge have been metals
(Alonso et al., 2009; Arif et al 2018; Černe et al., 2019), pesticides
(Xu et al., 2018), polycyclic aromatic hydrocarbons (Mailler et al.,
2014) and those included in the list of priority organic pollutants
(Directive 39/2013/CE). Nevertheless, the information about the
occurrence and fate of emerging concern pollutants in sludge treat-
ment technologies is scarce and mainly focused on anaerobic diges-
tion treatments (Stasinakis et al., 2012; Stasinakis et al., 2013).
Moreover, only a few papers have compared the occurrence and
fate of certain groups of emerging concern pollutants, such as sur-
factants (González et al., 2010; Cantarero et al., 2012), the plasti-
ciser bisphenol A (Guerra et al., 2015), pharmaceuticals (Martín
et al., 2012; Martín et al., 2015) and the biocide triclosan (Tohidi
et al., 2017), in different sludge treatment technologies.
Therefore, the aims of this work were i) to determine the occur-
rence and fate of six groups of endocrine disrupting compounds
(Table S1) in sludge from anaerobic and aerobic treatment plants,
composting plants and anaerobic stabilization ponds; ii) to com-
pare the influence of the stabilization technologies on the concen-
trations of the target pollutants; iii) and to evaluate the potential
environmental risks in treated sludge and in treated sludge-
amended soils.
2. Materials and methods
2.1. Chemicals and reagents
HPLC-grade acetonitrile (ACN), methanol (MeOH) and water
were supplied by Romil (Barcelona, Spain). Analytical-grade
ammonium acetate (98%) was provided by Panreac (Barcelona,
Spain). Glacial acetic acid (HAc) was supplied by Scharlab (Barce-
lona, Spain). High purity standards of methylparaben (MeP), ethyl-
paraben (EtP), propylparaben (PrP), benzylparaben (BzP),
triclocarban (TCB), triclosan (TCS), bisphenol A (BPA),
benzophenone-1 (BP-1), benzophenone-2 (BP-2), benzophenone-
3 (BP-3), benzophenone-6 (BP-6), benzophenone-8 (BP-8), 4-
hydroxybenzophenone (4-OH-BP), perfluorobutanoic acid (PFBuA),
perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA),
perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA)
and perfluorooctanesulfonic acid (PFOS) were supplied by Sigma-
Aldrich (Steinheim, Germany). Sodium dodecylsulfate (AS-C12),
sodium tetradecylsulfate (AS-C14), sodium hexadecylsulfate (AS-
C16) and sodium octadecylsulfate (AS-C18) were supplied by Alfa
Aesar (Barcelona, Spain). The chemical structures and physical–
chemical properties of the target compounds are shown in
Table S1. Isotopically-labelled compounds, used as internal stan-
dards (I.S.), were supplied by Sigma-Aldrich (Steinheim, Germany)
(EtP-d5, BP-d10, and BPA-d16) and by Cambridge Isotope Laborato-
ries (MA, USA) (PFOA-13C4). C18 sorbent was provided by Scharlab
(Barcelona, Spain). Individual stock solutions of each compound
were prepared at 1000 lg mL1 in MeOH and stored at 18 °C.
Working solutions were prepared by diluting the stock standard
solutions in MeOH.
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
2.2. Sample collection and stabilization treatments
Sludge samples were collected from four AnTPs, one CP, two
AeTPs and three AnSPs located in the South of Spain. In Fig. 1, it
can be seen treatment lines and types and characteristics of sludge
sampled from each treatment plant. Characteristics of each plant
can be seen in Table S2. Primary sludge (PS), secondary sludge
(SS), mixed sludge (MS), anaerobically-digested and dehydrated
sludge (AnDS)), aerobically-digested and dehydrated sludge
(AeDS)) and composted sludge (CS) were monthly collected.
Lagoon sludge (LS) was collected twice in a year, in January and
in August, because of the high residence time of sludge in AnSPs
(1–2 years) in comparison to the other types of sludge (1 month
approximately). PS and SS were introduced in the same proportion
in the anaerobic digestor. After digestion and dehydration, the
AnDS generated in the four AnTPs were composted in the same
CP by means of dynamic batteries thermally-controlled with aera-
tion provided by turning. Two litres of PS, SS, MS, and LS and 1 kg of
AnDS, AeDS and CS were collected in glass bottles. Samples were
freeze-dried in a Cryodos-50 lyophilizer (Telstar, Terrasa, Spain),
homogenized, crushed with a mortar and sieved (particle size
<100 mm). When necessary, they were kept in glass bottles and
maintained at 18 °C until analysis.
2.3. Analytical determination
The analytical determination was carried according to a previ-
ously reported method (Abril et al., 2018). The method consisted
on ultrasound-assisted extraction with 3 mL of MeOH:HAc (95:5,
v/v), clean-up by dispersive solid-phase extraction (d-SPE) with
0.8 g of C18 and analytical determination by liquid
chromatography-tandem mass spectrometry (LC-MS/MS). Chro-
matographic analysis was performed using an Agilent 1200 series
HPLC (Agilent, USA) coupled to a 6410 triple quadrupole (QqQ)
mass spectrometer (MS) equipped with an electrospray ionization
source (ESI). Chromatographic separation was carried out with a
HALO C18 column (50 mm  4.6 mm i.d., 2.7 mm particle size)
(Advanced Materials Technology, USA) protected with a HALO
C18 guard column (4.6  5 mm, 2.7 m particle size (Advanced
Materials Technology, USA) and thermostated at 25 °C. Mobile
phase was composed by a 10 mM ammonium acetate aqueous
solution and ACN. Gradient elution was carried out at a flow rate
of 0.6 mL/min by a linear increase from 30% to 70% of ACN in
14 min; then to 80% ACN in 5 min, held for 6 min, and back to ini-
tial conditions by a linear decrease of ACN proportion from 80% to
30% in 1 min, held for 5 min for re-equilibration. The injection vol-
ume was 10 mL. MS parameters were as follows: capillary voltage,
3000 V; drying gas flow rate; 9 L/min; drying gas temperature;
350 °C; and nebulizer pressure; 40 psi. Detailed information on
LC-MS/MS and method validation parameters can be found in
Tables S3 and S4, respectively.
2.4. Quality control
Procedural blanks and a matrix-matched calibration standard at
a medium concentration level (100 ng g1 for each target com-
pound) were injected every 10 samples in each batch of samples.
2.5. Ecotoxicological risk assessment
Environmental risk assessment was carried out using risk quo-
tients (RQ) according to the European Commission Technical
Guideline Document (EC-TGD, 2003). RQ value for each compound
in sludge was calculated as the ratio between its measured envi-
ronmental concentration (MEC) and its predicted no-effect concen-
tration (PNEC). The RQs for sludge-amended soils were calculated
 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx
Fig. 1. Sludge stabilization treatments and location of sampling points.
from the predicted environmental concentration (PEC) calculated
from the equation. Eq. (1) (EC-TGD, 2003):
PEC soil ¼ MEC sludge APPLsludge =DEPTHsoil RHOsoil
where MECsludge is the concentration (ng/g dm) of the organic pol-
lutant measured in sewage sludge; APPLsludge is the sludge applica-
tion rate (0.5 kg m2 for agricultural soils); DEPTHsoil is the mixing
depth (0.20 m for agricultural soils); and RHOsoil is the bulk density
of wet soil (1700 kg m3 for agricultural soils). PNECsoil were calcu-
lated from the PNECwater value and soil-water distribution coeffi-
cient (Kd) of each pollutant calculated from EC50. More
information about PNECsoil calculation and calculated PNECsoil val-
ues can be found in Table S5. Risk levels were categorised from
RQ values as: low risk (RQ values from 0.01 to 0.1), medium risk
(RQ values between 0.1 and 1) and high risk (RQ values higher than
1) (Ding et al., 2018; Mungray et al., 2008).
3. Results and discussion
3.1. Distribution of organic pollutants in the evaluated sludge
stabilization treatments
The occurrence and fate of each group of pollutants in each type
of sludge are shown as box-and-whisker plots in Fig. 2. Lines in
each box correspond to the lower (5%), median (50%) and upper
percentile (95%). The point inside each box shows the mean con-
centration whereas lines extending from each end of the box show
the maximum and minimum concentration values. The highest
mean concentrations in untreated sludge corresponded to the
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
3
anionic surfactants AS-C12 (1318 ng/g dm in PS, 3590 ng/g dm in
MS, 2851 ng/g dm in AeDS and 2133 ng/g dm in LS) and AS-C18
(2361 ng/g dm in SS and 1027 ng/g dm in CS). In AnTPs, the highest
ð1Þ mean concentrations of some groups of compounds, such as sur-
factants and biocides, were measured in SS (sum of mean concen-
trations: 6210 ng/g dm and 190 ng/g dm, respectively) whereas the
highest mean concentrations of other groups, such as PFCs, and
BPA, were measured in AnDS (sum of mean concentrations:
365 ng/g dm and 245 ng/g dm, respectively) (Fig. 2). In addition,
as indicate the dash arrows in Fig. 2, the concentration of the sur-
factants and biocides decreased after anaerobic digestion (from
4331 ng/g dm (PS-SS mean value) to 964 ng/g dm (AnDS) and from
117 ng/g dm (PS-SS mean value) to 89 ng/g dm (AnDS), respec-
tively) and increased after aerobic digestion in AeTPs (from
4790 ng/g dm (MS) to 7111 ng/g dm (AeDS) and from 7.0 ng/g
dm (MS) to 94 ng/g dm (AeDS), respectively) whereas the concen-
trations of PFCs and BPA increased after anaerobic digestion (from
207 ng/g dm (PS-SS) to 365 ng/g dm (AnDS) and from 72 ng/g dm
(PS-SS) to 245 ng/g dm (AnDS), respectively) and remained con-
stant after aerobic digestion (from 270 ng/g dm (MS) to 272 ng/g
dm (AeDS) and from 30 ng/g dm (MS) to 44 ng/g dm (AeDS),
respectively) (Fig. 2). These facts can be explained, as described
in detail in sections below, not only by a removal of the target com-
pounds by the sludge treatment applied but also to their different
sorption behaviour. Sorption onto sludge can be due to hydropho-
bic interactions and to electrostatic interactions that are condi-
tioned by log Kow and pKa values of the target compounds (data
in Table S1), and organic matter content (OM) and pH of sludge
(data in Fig. 1) (Verlicchi et al., 2015). For instance, the higher con-
centrations of surfactants and biocides in SS than in PS can be
4 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx

AnTP CP AeTP AnSP

8000
Concentration (ng/g dm)
Anionic
surfactants
6000

4000

2000

1000
Concentration (ng/g dm)

Biocides
800

600

400

200

1500
UV-Filters
Concentration (ng/g dm)

1000

500

600
Preservatives
Concentration (ng/g dm)

450

300

150

0
600
PFCs
Concentration (ng/g dm)

450

300

150

600
BPA
Concentration (ng/g dm)

450

300

150

0
Primary Secondary Anaerobically Composted Mixed Aerobically Lagoon
sludge sludge digested and sludge sludge digested and sludge
dehydrated sludge dehydrated sludge

Fig. 2. Box-and-whisker plots of the concentrations of the pollutants in each sludge stabilization technology.

explained by their high log Kow values, in the range from preservatives (log Kow values in the range from 1.91 to 3.82) were
4.42 to 7.08 (Table S1), and the higher organic matter content of similarly retained in both types of sewage sludge. In addition, a
SS (79%) with respect to PS (67%) whereas UV-filters and strong sorption onto sludge can also affect the biodegradation of
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx
the pollutant by reducing its bioavailability and, consequently, can
result in an increase of the concentration of the most recalcitrant
compounds after sludge treatment. This fact could explain the
increase of the concentrations of PFCs and BPA after anaerobic
digestion and the increase of concentrations of anionic surfactants,
UV-filters after aerobic digestion (Fig. 2).
3.1.1. Anionic surfactants
The occurrence and fate of each anionic surfactant in each
sludge stabilization treatment are shown as box-and-whisker plots
in Fig. S1. The sum of mean concentrations of AS-C12, AS-C14, AS-
C16 and AS-C18 in non-treated sludge (fresh sludge) were 2452,
6210, 4790 and 7111 ng/g dm in PS, SS, MS and LS, respectively.
The distribution pattern of the surfactants in PS was similar to that
in MS (AS-C12 > AS-C14 > AS-C16 > AS-C18) (Fig S1) and consistent
with that used in detergent formulations (Kavitha et al., 2014;
Morrall et al., 2006). Nevertheless, in SS, the highest concentrations
corresponded to AS-C18 (mean value: 2639 ng/g dm). The different
distribution pattern in SS (AS-C18 > AS-C12 ffi AS-C14 ffi AS-C16)
could be explained by the higher organic matter content of SS
(78.0–84.2%) in comparison to PS (65.8–69.1%), MS (59.0–66.8%)
and LS (38.3–49.5%), what ease the sorption of AS-C18. AS-C18 is
the anionic surfactant with the highest log Kow value (7.08)
(Table S1). After sludge digestion, a different behaviour was
observed depending on the anaerobic or aerobic conditions of the
digestion process. Concentrations of the four anionic surfactants
decreased after anaerobic digestion (Fig. S1) but aerobic treat-
ments such as composting and, especially, aerobic digestion caused
a decrease of the concentrations of the shorter chain surfactant
(AS-C12) whereas the concentrations of AS-C14 were not affected
and the concentrations of the longer chain surfactants (AS-C16
and AS-C18) increased. In the case of LS, the high concentrations
(mean values: 2133, 1485, 617 and 924 ng/g dm for AS-C12, AS-
C14, AS-C16 and AS-C18, respectively) in comparison to PS, SS
and MS could be explained by the high sludge age of LS what ease
the accumulation of contaminants.
3.1.2. Biocides
The occurrence and fate of TCB and TCS in each type of sludge are
shown as box-and-whisker plots in Fig. S2. TCS was measured at
higher concentrations than TCB what can be explained by its higher
use in personal care products (Chen et al., 2019). Mean concentra-
tions of TCS in PS, SS, MS and LS were 64.2, 439, 7.0 and 22.1 ng/g
dm, respectively, while mean concentrations of TCB were 0.09,
2.27 and 0.22 ng/g dm in PS, SS and LS, respectively. TCB was not
detected in MS. Mean concentrations of TCS in AnDS, CS and AeDS
were 88 ng/g dm, 205 ng/g dm, and 93.4 ng/g dm, respectively.
Mean concentrations of TCB in AnDS, CS and AeDS were 1.4 ng/g
dm, 5.7 ng/g dm and 1.1 ng/g dm, respectively. The concentrations
of TCS in this work are higher than those reported by Lehutso et al.
(2017) in non-treated sludge (TCS: 3.65–15 ng/g and TCB: 3.65–1
1.8 ng/g) and in treated sludge (TCS: 2.1–7.8 ng/g and TCB: 1.2–
9.2 ng/g) from South Africa but much lower than those reported
in sludge from China by Chen et al. (2019) (TCS: 4–4870 ng/g dm
and TCB: 3–43300 ng/g dm) and Yu et al. (2011) (TCS: 1188 ng/g
dm; TCB: 5088 ng/g dm). This variability can be explained by the
different consumption pattern of personal care products where
TCB and TCS are used as antimicrobial agents. The higher concen-
trations of TCB and TCS in SS (2.3 and 439 ng/g, respectively) than
in PS (0.09 and 64.2 ng/g) can be due to the higher organic matter
content of SS what ease their sorption as described above for anio-
nic surfactants. TCS was detected in 95% of the SS samples at con-
centrations up to 426 ng/g dm. Concentrations of TCS and TCB
increased from AnDS to CS and from MS to AeDS (Fig. S2). For
instance, TCB was not detected in MS but was detected in 20% of
AeDS samples at concentrations from 2.64 to 7.20 ng/g dm. The
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
5
above-mentioned increase of concentrations could be explained
by a poor removal of the TCB and TCS (recalcitrant compounds)
under aerobic conditions (composting and AeD) together with the
loss of weight of treated sludge by the removal of organic matter.
3.1.3. UV filters
In Fig. S3 are shown box and whisker plots of the concentrations
of the UV filters in sludge from AnTs, CPs, AeTs and AnSPs. BP-3
was the UV filter most frequently detected (in 95% of the analysed
samples) whereas BP-6 and BP-8 were not detected in any of the
analysed samples. The highest concentrations of UV filters corre-
sponded to BP-3 and 4-OH-BP in PS (509 ng/g dm and 792 ng/g
dm, respectively), to BP-3 in SS (669 ng/g dm) and to 4-OH-BP in
AeDS (1089 ng/g dm). BP-3 has a high log Kow value (log Kow:
3.79) what can explain its high sorption onto sludge whereas 4-
OH-BP has been reported to be the most abundant benzophenone,
with the highest concentrations, in influent wastewater (Wang
et al., (2017)). Moreover, 4-OH-BP can be also generated by
alkylphenol degradation, by the transformation of BP-3 into 4-
OH-BP in influent wastewater and by its excretion as a human
metabolite of BP-3 (Wang and Kannan, 2017). As can be seen in
Fig. 2, the sum of UV-filters decreased from PS (mean: 292 ng/g
dm) and SS (mean: 161 ng/g dm) to AnDS (mean: 45 ng/g) and
CS (mean: 26 ng/g dm). Nevertheless, in AeTPs it was observed
an increase of the concentrations of the sum of UV-filters from
393 ng/g dm in MS to 637 ng/g in AeDS. Sum of UV-filters in LS
(463 ng/g) were similar to that measured in PS, SS and MS.
3.1.4. Preservatives
As can be seen in Fig. 2, the highest concentrations of parabens
were found in sludge from AnSPs (mean concentration for the sum
of MeP, EtP, PrP and BzP: 287 ng/g dm). In spite of the low log Kow
values of the parabens (from 1.91 to 3.59) all of them, except EtP,
were detected in all the types of sewage sludge analysed (Fig. S4).
EtP was not detected in sludge prior digestion but was detected in
two AnDS samples (69 ng/g dm and 55 ng/g dm). This fact could be
explained by its persistence to degradation together with the loss
of weigh of sewage sludge by the removal of organic matter result-
ing in an increase of the concentration after sludge digestion. Con-
centrations measured in this work are similar to those found in
other studies carried out in Spain by Nieto et al. (2009) (MeP:
46–202 ng/g dm; EtP: not detected (nd); PrP: 6–7 ng/g dm; BzP:
nd-5 ng/g), and in Korea by Liao et al. (2013) (MeP: 4.31–540 ng/
g dm; EtP: nd-2.12 ng/g dm; PrP: nd-32.5 ng/g; BzP: nd-2.89 ng/
g dm). The distribution pattern is similar to that reported by
Núñez et al. (2008) in sediments and agricultural soils from Spain
(MeP: 0.63–1.80 ng/g dm; EtP: 0.59–1.17 ng/g dm;PrP:
0.59–2.20 ng/g dm; BzP: nd-1.83 ng/g dm); by Lee et al. (2005)
in influent (MeP: 0.10–1.47 ng/mL; EtP: 0.02–0.27 ng/mL; PrP:
0.2–2.43 ng/mL; BzP: 0.02–0.26 ng/mL) and effluent sewage sludge
(MeP: 0.02–0.03 ng/mL; EtP: nd; PrP: nd-0.04 ng/mL; BzP:
nd-0.01 ng/mL) from Canada and in wastewater (González-
Mariño et al., 2011; Ma et al., 2018; Molins-Delgado et al., 2016;)
in Guadiamar River basin in Spain (Garrido et al., 2016) and with
their use in cosmetics and in food industry).
After anaerobic digestion and composting, the concentrations of
MeP and BzP decreased (MeP: from 38.5 ng/g dm in the mixture
PS-SS to 26 ng/g in AnDS and 11 ng/g in CS; BzP: from 26.5 ng/g
dm in the mixture PS-SS to 9 ng/g in AnDS and 6 ng/g in CS)
whereas the concentration of PrP slightly increased (from
21 ng/g dm, in the mixture PS-SS, to 25 ng/g in AnDS and
38 ng/g in CS) (Fig S4). However, after aerobic digestion, the sum
of the concentrations of parabens in AeDS (mean: 120 ng/g dm)
was slightly higher than that in MS (mean: 72 ng/kg dm) being
PrP and BzP the parabens with a higher increase from MS to AeDS
(PrP: from 36 ng/g dm in MS to 52 ng/g dm in AeDS; BzP: mean
6 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx

Preservatives PFCs Biocides BPA Anionic surfactants UV-Filters

100000,00
AnDS
10000,00

1000,00

100,00
Risk quotient

10,00

1,00

0,10

0,01

0,00

0,00
10000,00
AeDS
1000,00

100,00
Risk quotient

10,00

1,00

0,10

0,01

0,00

0,00

100000,00
Composted Sludge
10000,00

1000,00

100,00
Risk quotient

10,00

1,00

0,10

0,01

0,00

0,00

1000,00
Lagoon Sludge
100,00

10,00
Risk quotient

1,00

0,10

0,01

0,00

0,00

Fig. 3. Risk quotients (RQ) for treated sludge calculated from measured concentrations in sludge.

from 24 ng/g dm in MS to 61 ng/g dm in AeDS). The increase of together with a removal of the organic matter content of sludge
concentrations of PrP and BzP after composting and after AeD resulting in an enhancement of the concentration of the parabens
could be explained by a poor degradation under aerobic conditions in aerobically-treated sludge.
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx 7

Preservatives PFCs Biocides BPA Anionic Surfactants UV-Filters

100,00
AnDS-amended soil

10,00
Risk quotient

1,00

0,10

0,01

0,00

0,00

10,00
AeDS-amended soil
Risk quotient

1,00

0,10

0,01

0,00

0,00
100,00
Composted sludge-amended soil
Risk quotient

10,00

1,00

0,10

0,01

0,00

0,00
10,00
Lagoon sludge-amended soil
Risk quotient

1,00

0,10

0,01

0,00

0,00

Fig. 4. Risk quotients (RQ) for treated sludge-amended soils.

This fact contrasts with the better degradation of MeP and PrP in this work are consistent with the stability of MeP and PrP in
under experimental aerobic conditions than under anaerobic con- sludge reported by Li et al. (2015). The highest concentrations of
ditions reported by Wu et al. (2017). However, the results obtained PrP and BzP were found in LS, in spite of the low volume of
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
8 C. Abril et al. / Science of the Total Environment xxx (xxxx) xxx
wastewater treated in AnSPs. This fact can be explained by the high
residence time of sludge in AnSP what promotes the accumulation
of these compounds.
3.1.5. Perfluoroalkyl compounds
The sum of mean concentrations of PFCs were up to 487, 446
and 299 ng/g dm in PS, SS and MS, respectively. A similar distribu-
tion pattern was found in all types of sludge
(PFHxA > PFHpAPFPeA > PFBuA > PFOA > PFOS) (Fig. S5). In spite
of the wide variability in PFC concentration reported from a sew-
age treatment plant to another (Arvaniti and Stasinakis, 2015;
Campo et al., 2014) and from a sampling campaign to another
(Campo et al., 2014), the distribution pattern in this work, except
for PFOS and PFOA, is consistent with the higher tendency of longer
PFCs to be sorbed onto sludge described by Arvaniti et al. (2015).
Concentrations for PFOS and PFOA in this work are lower than
those of shorter chain PFCs but are within the ranges from 5 to
160 ng/g dm and from 1 to 241 ng/g dm reported by Clarke and
Smith (2011) for PFOS and PFOA, respectively, in three sludge
treatment plants in USA and in another from Denmark. As can be
seen in Fig S5, PFC concentrations increased after AnD and were
maintained constant after AeD. This fact is consistent with the high
stability provided by the extremely strong carbon-fluorine bonds
in their chemical structures (Table S1) (Arvaniti and Stasinakis,
2015). Composting caused a decrease of the concentrations of per-
fluoroalkyl carboxylic acids but produced an increase of the con-
centrations of PFOS (Fig. S5). The increase of PFOS concentration
after composting could be due to a poor degradation under aerobic
conditions together with high decrease of organic matter content
of sludge by composting.
3.1.6. BPA
Concentrations of BPA in treated sludge were up to 579, 658
and 77 ng/g dm in AnDS, CS and AeDS, respectively (Fig. 2). BPA
concentration increased after AnD (mean concentrations in PS, SS
and AnDS: 45 ng/g dm, 100 ng/g dm and 245 ng/g dm, respec-
tively) but decreased, or was maintained constant, after compost-
ing (from 245 ng/g in AnDS to 187 ng/g in CS) and AeD (from
30 ng/g dm in MS to 44 ng/g in AeDS) (Fig. 2). This fact reveals a
poor degradation under anaerobic conditions and better degrada-
tion under aerobic conditions what allows maintaining its concen-
trations similar to those prior sludge treatment. These results are
consistent with the poor removal rates of BPA in AnTPs reported
by Samaras et al. (2013). The concentrations of BPA in this work
are within the range from 4 ng/g dm to 1750 ng/g dm reported
by Clarke and Smith (2011) in sewage sludge samples from
Germany, Australia, Greece and China but lower than those
reported by Petrie et al. (2019) in digested sludge from two
treatment plants affected by industrial BPA discharges (4600 ng/g
dm-38700 ng/g dm).
3.2. Environmental risk assessment
The ecotoxicological risk was evaluated at two possible scenar-
ios: the ecotoxicological risk in treated sludge generated in each
stabilization treatment and the risks associated to treated-sludge
application onto agricultural soils. In Fig. 3 and Fig. 4, it can be seen
box and whisker plots representing RQ values corresponding to
treated sludge and to treated sludge-amended soils, respectively.
All the compounds, except TCB and AS-C18, imply ecotoxicological
risk (mean RQ > 1) in sludge (Fig. 3). but, after sludge application
onto soil, the ecotoxicological risks decreased to RQ values lower
than 1, except for TCS (Fig. 4). RQ values higher than 1 were
obtained for TCS in 40, 40, 50 and 5% of AnDS, AeDS CS and LS anal-
ysed samples. A high ecotoxicological risk due to 4-OH-BP was
obtained after application onto soils of 95% of AeDS samples.
Please cite this article as: C. Abril, J. L. Santos, J. Martín et al., Occurrence, fate and environmental risk of anionic surfactants, bisphenol A, perfluorinated
compounds and personal care products in sludge stabilization treatments, Science of the Total Environment, https://doi.org/10.1016/j.
scitotenv.2019.135048
The obtained results are consistent with the scarce information
about environmental risks reported for treated sludge-amended
soils. For instance, Thomaidis et al. (2016) reported RQ > 1 for
TCS and RQ < 1 for PFOS and PFOA in AnDS-amended soils.
Verlicchi and Zambello (2015) also reported RQ > 1 for TCS in
sludge-amended soils. In spite of the low RQ values obtained for
PFCs, they have been reported to be persistent in soils (>6 months),
to be ecologically bio accumulative and to probably enter into the
human food chain (Clarke and Smith, 2011). On the other hand, the
persistence in soils of other compounds such as TCS and TCB is
uncertain although there are evidences of their ecological bioaccu-
mulation and soil ecotoxicity (Clarke and Smith, 2011).
4. Conclusions
The highest concentrations in untreated sludge were measured
in SS and corresponded to anionic surfactants. Anionic surfactants
were also the compounds at the highest concentration levels in all
types of sludge. After anaerobic digestion, the concentrations of
surfactants, biocides, UV-filters and preservatives were similar to
that in untreated sludge whereas the concentrations of PFCs and
BPA increased. Nevertheless, composting decreased the concentra-
tions of such compounds (84% for PFCs and 23% for BPA). An
increase of concentrations, in the range from 31 to 40%, except bio-
cides (92%), was also observed for all the groups of compounds,
after aerobic digestion. Different behaviour was observed for com-
pounds belonging to the same group what could be explained by
their different log Kow values what conditions their sorption onto
sludge and, therefore, their bioavailability for degradation. Envi-
ronmental risk assessment revealed environmental risk in treated
sludge for 21 out of the 23 target compounds. This fact could
involve negative effects on microorganisms responsible of sludge
digestion treatments. Environmental risks in treated sludge-
amended soils were limited to TCS in soils amended with AnDS,
AeDS and CS and to 4-OH-BP in soils amended with AeDS.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.scitotenv.2019.135048.
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