Volume 9 - 2021 | https://doi.org/10.3389/fenvs.2021.715772
This article is part of the Research TopicMicropollutants in the Aquatic EnvironmentView all 6 articles
The concentrations of 25 pharmaceuticals and endocrine disruptors were monitored in the water coming from the Tibagi River (State of Paraná
Brazil) and in a conventional water treatment plant over 13 sampling campaigns
dexamethasone and losartan) were detected with high frequency (>75%) and 4 drugs (estradiol
loratadine and naproxen) were found with moderate frequency (between 30 and 70%)
benzafibrate and promethazine) were not detected in any of the samples analyzed and 11 other compounds were quantified at low frequency (up to 25%)
The conventional treatment process employed at WTP- Jataizinho has proven to be very efficient in removing dexamethasone (∼99%)
moderately efficient in reducing bisphenol A (∼47%) concentration and inefficient in removing losartan (∼22%) and loratadine (not removed)
The greatest removals were observed during the water clarification stage using aluminum sulfate as coagulant
the dry and rainy seasons did not influence the concentrations of pharmaceuticals and endocrine disruptors in raw water
In terms of the 5 most prevalent micropollutants in treated water (bisphenol A
the human health risk associated with ingesting contaminated water was assessed and considered negligible
In Brazil, Machado et al. (2016) analyzed 100 samples of DW, collected in 22 Brazilian State capitals, and 7 of these samples came from surface springs. Caffeine and atrazine were the most frequently detected micropollutants, both in springs and in public water supply. In turn, Reis et al. (2019) analyzed 28 drugs
in superficial springs and water treatment plants (WTPs) in the State of Minas Gerais
Eighteen drugs were detected in superficial springs and 11 in treated water
The concentrations in the treated water were lower than those present in the springs
thus demonstrating that at least part of the contaminants can be removed in conventional treatment
that the clarification step accounted for only 15% of the removal
while disinfection (32%) and filtration with activated carbon (53%) were more efficient
this work aimed to analyze the presence of 25 drugs and endocrine disruptors in raw water (RW) of the Tibagi River
to verify the removal of these compounds in the conventional treatment plant in the city of Jataizinho (PR) in 13 sampling campaigns during the dry and rainy seasons
it has been evaluated whether the remaining concentration of these compounds in the treated water poses significant risk to the human health
The hypothesis behind these objectives is that although Brazilian rivers are polluted with contaminants of emerging concern due to the discharge of sewage (raw or partially treated)
the technologies employed in the WTP can reduce the concentration of such compounds to levels deemed safe for human health
The average annual rainfall of the basin varies between 1,200 mm and 1900 mm (IAPAR-EMATER, 2018)
The distribution of the average monthly precipitation values shows regularity along the basin and a period of low precipitation between the months of April and August (dry period)
while the maximum expected is around 112 mm
During the months of September to March (rainy period)
the average and minimum values are 149 and 111 mm
close to the maximum expected for the dry period
Sewage collection and treatment systems in the Tibagi River basin cover 82% of the urban population and 54 WWTPs are in operation. Near the collection point used in this study (20 km upstream of the city of Jataizinho), the Tibagi river receives treated sewage from four WWTPs located in southern Londrina, with a total average flow of 670 L/s (Figure 1.)
Map of Tibagi river basin and Tibagi River location indicating: 1) Sewage treatment plants (23o21′23´´ e 51o07′03´´; 23o21′52´´e 51o07′11´´
23o22′43´´e 51o10′37´´
23o24′02´´e 51o07′54´´) 2) Tibagi river collection point and (23o28′43´´,50o59′43´´) 3) the Jataizinho water treatment plant (23o15′33´´ e 50o58′38´´)
the WTP operates at a flow rate of 60 L s−1
resulting in operating times between 10 and 14 h per day (intermittence in water production)
the station operates with less interruptions in the morning
it was chosen to collect four 500 ml aliquots
to make up a 2 L composite sample during such period
RW samples were collected in the inlet channel
using a 500 ml graduated glass cylinder
previously prepared (washed with 10% nitric acid)
the glass cylinder was washed with RW for five times
Each aliquot (500 ml) was added to a 2-L glass container and kept under refrigeration
the filtered water is directed through a closed pipe to the contact chamber
pumps were installed that take the FW through pipes to the operational and quality control laboratory
The filter chosen for sampling was the one that had been washed a short time ago
then the graduated cylinder was washed five times with FW
and a volume of 500 ml was collected to constitute the composite sample
Each aliquot (500 ml) was added to a 2-L glass container and kept under refrigeration (4°C)
Samples of the filter washing water (FWW) were collected in the outlet channel of the washing water
the initial outlet water was discarded (1–2 min) and a sample (approximately 2 L) of the washing water was collected
The collection of DW was performed through a tap
which receives treated water from the raised reservoir
then the graduated cylinder was washed five times with the DW and a volume of 500 ml was collected to constitute the composite sample
The methods described in Standard Methods for the Examination of Water and Wastewater, 22nd edition (APHA, AWWA, WEF, 2012), indicated in Table 1
were used to perform physicochemical characterization of water samples collected at WTP- Jataizinho
Parameters and methods used for the physicochemical analysis of the water collected at Jataizinho WTP
The analyses of pharmaceuticals and endocrine disruptors were based on the work of Corrêa et al. (2021) and Sanson. (2012)
developed at the Laboratory of Molecular Characterization and Mass Spectrometry (LABMASSAS) of Universidade Federal de Ouro Preto (UFOP)
the water samples collected in composed form immediately underwent vacuum filtration processes using fiberglass membranes of different porosities (8 μm
followed by 2 and 0.45 µm) for the removal of particulate material
The SPE cartridges containing the compounds of interest were identified and stored in a freezer for subsequent sending to the LABMASSAS of UFOP
In LABMASSAS the SPE cartridges were submitted to the elution of the analytes using 9 ml of ethyl acetate in a 12-port vacuum manifold
the resulting extracts were dried with gaseous nitrogen by means of a concentrating apparatus that maintained the extract at room temperature during drying
The vials containing the dried extracts were kept in a freezer until analysis
Retention times and mass/charge ratios (m/z) of micropollutants analyzed by GC-MS
The response used to construct the analytical curves was the ratio of analyte peak area to internal standard peak area (IS) (y-axis) against analyte concentration (x-axis). Thus, for the samples, the ratio between the areas of the analyte and IS was also used. Eq. (1) was used for the evaluation of the matrix effect (ME)
in which Aspike is the area of the analyte in the spike vial
A is the area of the analyte in the sample vial and in the denominator is represented the area of the analyte at 30 μg L−1 according to the equation of the analytical curve
The same extracts obtained in item 2.4 after redissolving the SPE extract in 500 µL of HPLC grade methanol (J.T
was transferred (100 µL) to a vial containing a volume restrictor
This extract was then dried under nitrogen gas flow and kept in a freezer (−26°C) until analysis
stock solutions in methanol HPLC grade (J.T
sulfamethoxazole and naproxen) were prepared in 1 g L−1 concentration
The working solutions containing all the analytes were prepared from these solutions at a concentration of 1 mg L−1
in methanol and containing all the analytes
dilutions were made with methanol containing 0.1% v/v formic acid (88%
Baker) from the working solution on the day of analysis with a concentration range of 2.5–50 μg L−1
vial named standard solution (Astandard) were prepared
containing standard solution in methanol with 0.1% v/v formic acid with all the analytes at a concentration of 30 μg L−1
and the vial named solvent (Asolvent) containing only methanol with 0.1% v/v formic acid
the vials containing the dry extract were redissolved with 100 µL of methanol with 0.1% v/v formic acid
The analyses were performed using the LCMS-8040 equipment (Shimadzu) coupled with the UHPLC model Nexera (Shimadzu) with the following modules: CBM-20A controller
A C18 chromatographic column model Kinetex (Phenomenex) 100 mm × 2.1 mm × 2.6 µm was used
The mobile phase consisted of 1) ultrapure water with 0.1% v/v formic acid; 2) acetonitrile (HPLC grade
using the following gradient steps of solvents: 5% B from 0 to 1 min
rising to 95% B at 13 min and returning to the initial condition at 14 min
This resulted in a total running time of 16 min under a flow rate of 0.250 ml min−1
acetonitrile solution containing 3.5 mM ammonium hydroxide (28%
was subsequently added post column at a flow rate of 0.03 ml min−1
data were treated considering the recovery percentage of each analyte
The matrix effect was corrected using the ratio as a response
the correction of the effect was punctual in relation to the sample and the analyte
Mass/charge ratio (m/z) of precursor and products monitored in LC/MS in Multiple Reaction Monitoring (MRM) mode
The MOE represents whether the occurrence of the compound in question is lower or higher than its guide value
and was used for risk classification as follows: 1) MOE ≤1 (imminent risk) for micropollutants in treated water at concentrations higher than or equal to the guide values and therefore pose health risks; 2) 1 < MOE <10 (high risk) for micropollutants found in treated water in concentrations lower than the guide values
but in the same order of magnitude as the concentrations which would represent health risks; 3) 10 < ME ≤ 100 (moderate risk) for micropollutants occurring in treated water in concentrations lower than the guide values in up to two orders of magnitude; 4) 100 < ME (low risk) for micropollutants found in treated water at concentrations at least one hundred times lower than the guide values
Where: MOE is the margin of exposure; GV is the guide value (calculated by Eq. 4 using the lowest tolerable daily intake value reported in the literature) and OC is the occurrence of the micropollutant in treated water (in this work the 95th percentile of the concentration of the pharmaceutical/endocrine disruptor in treated water was considered)
Where: TDI is the tolerable daily intake (μg/kg/d), derived from epidemiological or toxicological studies and, in the case of drugs. The TDI can be estimated by the therapeutic doses reported by manufacturers or pharmacopoeias considering an uncertainty factor, as presented in Eq. 5; BW means body weight (60 kg for the Brazilian population); AF means allocation factor (proportion of TDI attributed to water intake
which varies according to the contaminant) and V is the daily average water consumption (2 L/d for the Brazilian population)
Where: MDTD means the minimum daily therapeutic dose (mg d−1) and UF is the uncertainty factor (EPHC NHMRC NRMMC, 2008)
The TDI values used in the risk assessment performed in this work were obtained from the compilation presented by (Brandt et al., 2019)
as well as the number of micropollutants with concentrations above the limit of detection for each sample
Physicochemical quality parameters of Tibagi River water samples
Supplementary Figure S1 shows the average monthly precipitation values at the IAPAR Station
It can be noticed a clear difference in the average monthly precipitation between dry and rainy periods
It was found that the average monthly flow of the Tibagi River was 582 m3 s−1 during the rainy period and 251 m3 s−1 in the dry period
The concentrations of pharmaceuticals and endocrine disruptors detected in RW supplying WTP-Jataizinho is shown in the Supplementary Table S1
of the 25 pharmaceuticals and endocrine disruptors analyzed
in 67% of the samples they were not detected or were found with low frequency (in up to 23%)
The seven microcontaminants which were not detected in RW were: paracetamol
dexametazone (DXM) and losartan (LST)) were detected with a high frequency (above 77%) and four pharmaceuticals (estradiol
naproxen (NPX)) were found with moderate frequency (between 30 and 69%)
Among the five most prevalent substances in RW
only the endocrine disruptor BPA (chemical input used in the manufacture of resins and plastics) is not a pharmaceutical
being the four pharmaceuticals belonging to the classes of steroidal (DXM) and non-steroidal (NPX) anti-inflammatories
antihypertensive (LST) and antihistamine (LRT)
The concentrations of the 5 microppolutants mostly detected in the different collection points in the WTP are presented in Table 5
It is seen that dexametazone and naproxen occurred in higher concentrations in RW during the dry season when compared to the rainy season
while for the other compounds the differences observed were not statistically significant
Values of median concentrations of the 5 micropollutants most frequently detected in the dry (_D) and rainy (_R) periods in raw water (RW)
filtered water (FW) and drinking water (DW) of WTP-Jataizinho
Table 6 depicts endocrine disruptors and pharmaceuticals that have been quantified in at least 30% of the filter washing water (FWW) samples over the 13 sample campaigns
Out of the 8 compounds meeting this criterion
diclofenac and dexamethasone) occurred in the FWW at a median concentration equal to half the limit of detection (criterion normally used to replace < LOD by numerical values) of the analytical method
The BPA and naproxen compounds were found in the FWW in median concentrations higher than those observed in DW
while for loratadine and losartan compounds no significant differences in their median concentrations were observed in FWW and DW
Values of concentrations (ng L−1) of pharmaceuticals and endocrine disruptors which occurred in the filter washing water (FWW) of WTP-Jataizinho with a minimum frequency of 30%
During the dry period (March to September)
38 occurrences of micropollutants with concentration values above limit of detection (LOD) or limit of quantification (LOQ) were identified (6.3 per collection)
while during the rainy period there were 36 occurrences (5.1 per collection)
Analysis of data of the 3 compounds occurring with high frequency in the water of the Tibagi River indicated that there were no significant differences between the average concentrations calculated for the rainy and dry periods for the BPA (dry: 18.6 ng L−1; rainy: 17.3 ng L−1) and losartan compounds (dry: 3.3 ng L−1; rainy: 4.8 ng L−1)
whereas for dexamethasone compound (dry: 598.4 ng L−1; rainy: 182.6 ng L−1) the median concentration observed in the dry period was 3.3 times higher than that observed in the rainy period
This may suggest that the main source of such a corticoid input to the Tibagi River is the discharging of domestic sewage
therefore being more affected by the dilution factor caused by the increased river flowrate during the rainy season
Although sewage is more diluted in the rainy season
increased runoff can also contribute to diffuse pollution of the water body by carrying solid material containing micropollutants
veterinary drugs) and urban solid waste disposal (e.g
water quality monitoring data collected at the Chácara Ana Cláudia station
conducted by the Paraná Water Institute (AGUASPARANÁ)
indicated stable WQI values in the range of 52–69 throughout the monitoring period carried out on the Tibagi River
Analysis of principal components (PCA) of the contaminants present in the WTP-Jataizinho: (A) scores plot
The analysis of the score graph (Figure 2B) indicates a large dispersion of the micropollutants monitored and low correlation with the water quality indicator parameters which were widespread in the four quadrants of the PCA graph
the formation of a cluster including the parameters turbidity
bisphenol A and 4-octylphenol was clearly noted
These compounds are well-known endocrine disruptors of hydrophobic nature which tend to adsorb onto suspended organic matter that causes turbidity and apparent color
there was no significant apparent correlation between the parameters dissolved oxygen
For the parameter pH it was observed that it tended to cluster with six micropollutants of which four of them (DMX
the pH tended to cluster with compounds which exhibited no charge at neutral pH
except for NPX and GEN which are acidic compounds
Comparison of the concentration values of pharmaceuticals and endocrine disruptors, during dry and rainy periods, along the treatment stages used in WTP-Jataizinho were evaluated by the medians, as shown in Table 5. Figure 3 presents the changes in concentration along the treatment of the most prevalent compounds in WTP-Jataizinho
disregarding the separation between the dry and rainy periods
Changes in concentration (ng∙L−1) of the compounds most frequently detected in raw water at the WTP-Jataizinho: (A) bisphenol-A
It is important to highlight that a simple change in the structure of a given target compound would make its detection unfeasible in the developed method
the removal of a given microcontaminant was evaluated based on the reduction in the concentration of the target compound
disregarding the possible formation of related compounds
The high removal of dexamethasone at the clarification stage is somewhat surprising since such compound has moderate Kow and Koc values and
with greater affinity for water than for solids suspended therein
the removal in the clarification stage of about 35% of the BPA present in RW is consistent with its greater hydrophobicity and tendency to adhere to the flocs formed in the flocculator and retained in the decanter and filters of WTP-Jataizinho
it was observed that the more hydrophobic compounds (log Kow > 3) were present in the FWW
although some of them were not found with high frequency or concentration in RW or DW (used for filter washing)
This indicates that such compounds were probably removed preferably via adsorption to the flocs retained in the decanter and filter material
The presence of these compounds in the FWW possibly results from the desorption process due to the equilibrium displacement promoted by the use
of water containing lower concentration of hydrophobic contaminants retained in the flocs
The exception was dexamethasone (log Kow = 1.83)
which was repeatedly detected in the filter washing water and cannot be considered hydrophobic
the presence in the FWW probably arises from its frequent presence in the DW which was used to wash the filters
thereby indicating that the calculated risk is low
risk analysis performed here was quite conservative
it can be affirmed that the risk to human health would be negligible for the most prevalent pharmaceuticals and endocrine disruptors in the water treated by WTP-Jataizinho and future works should pay attention on the occurrence of dexametazone which
despite being efficiently removed by conventional treatment might exhibit adverse effects at concentrations as low as 25 ng L−1
The monitoring of 25 pharmaceuticals and endocrine disruptors carried out in the Tibagi River (Paraná/Brazil) over 13 sample campaigns comprising dry and rainy periods indicated that 7 micropollutants were not detected in any sample analyzed
DXM–dexamethasone and LST–losartan) were detected with a high frequency (> 10/13) in the RW
at median concentrations ranging from 17.3 ng L−1 (rainy) to 18.6 ng L−1 (dry) for BPA; 182.6 ng L−1 (rainy) to 598.4 ng L−1 (dry) for DXM; and 3.2 ng L−1 (dry) to 4.8 ng L−1 (rainy) for LST
There was no significant correlation between the micropollutants monitored and the usual water quality parameters although it was observed that the endocrine disrupters BPA and 4-nonylphenol (4NP) followed the behavior of turbidity and apparent color
The conventional treatment process (coagulation/flocculation/settling/sand filtration/chlorination) used on WTP-Jataizinho was very efficient in removing DXM (∼99%)
moderately efficient in removing BPA (∼47%) and not very efficient for LST removal (∼22%)
Despite the persistent presence of 5 microcontaminants (BPA
and NPX) in the treated water distributed to the population
the risk analysis carried out indicated that they occurred in concentrations (95th percentile) about 130–4,000 times lower than that which would cause some adverse effect
thus evidencing low risk of human exposure to such contaminants by the consumption of treated water
The original contributions presented in the study are included in the article/Supplementary Material
further inquiries can be directed to the corresponding author
All authors listed have made a substantial
and intellectual contribution to the work and approved it for publication
The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest
All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations
Any product that may be evaluated in this article
or claim that may be made by its manufacturer
is not guaranteed or endorsed by the publisher
The authors would like to thank the following agencies for their financial support: Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)
Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
Fundação Nacional de Saúde (FUNASA)
Universidade Federal de Ouro Preto (UFOP) and Universidade Tecnológica Federal do Paraná (UTFPR)
The Supplementary Material for this article can be found online at: https://www.frontiersin.org/articles/10.3389/fenvs.2021.715772/full#supplementary-material
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Received: 27 May 2021; Accepted: 31 July 2021;Published: 02 September 2021
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*Correspondence: Ananda Lima Sanson, YW5hbmRhX2xpbWFAdWZvcC5lZHUuYnI=
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SALT LAKE CITY (KUTV) — A missionary with The Church of Jesus Christ of Latter-day Saints has died and three others were injured after a bus crash in Brazil
Church officials said 20-year-oldElder Izaak Orion Card
died in the collision on Friday in a rural area near Tibagi
weretraveling on a bus in the early evening when it was hit by a semi truck
The other three missionaries did not sustain serious injuries and were being cared for by local members of the Church
Elder Card had been serving as a full-time missionary since October 2022
"We send our love to Elder Card’s family and friends and the missionaries and members in the Brazil Curitiba Mission," the Church said in a statement
"We pray that each will find peace and comfort as they mourn this faithful missionary and reflect on his Christlike service."
A tragic traffic accident in Brazil has claimed the life of a young missionary of The Church of Jesus Christ of Latter-day Saints
“Four missionaries were traveling on a bus in the early evening
when it was hit by a semitruck,” said Penrod in a Church statement
“The other missionaries did not sustain serious injury and are being cared for by local members of the Church.”
Elder Card has been serving as a full-time missionary in the Brazil Curitiba Mission since October 2022
“We send our love to Elder Card’s family and friends and the missionaries and members in the Brazil Curitiba Mission,” said Penrod
“We pray that each will find peace and comfort as they mourn this faithful missionary and reflect on his Christlike service.”
(The Church of Jesus Christ of Latter-day Saints) Elder Izaak Orion Card
A 20-year-old missionary with The Church of Jesus Christ of Latter-day Saints from Anchorage
a spokesperson for the faith said Saturday
Isaak Orion Card was riding the bus with three other missionaries in a rural area in Brazil, near the city of Tibagi, when the bus was hit by a semitruck, church spokesperson Sam Penrod said in a news release
The other missionaries weren’t seriously hurt
and are being taken care of by area Latter-day Saints
Card was serving in the Brazil Curitiba Mission
and he had been a full-time missionary since October
“We send our love to Elder Card’s family and friends and the missionaries and members in the Brazil Curitiba Mission,” the church said
This is the fourth publicly reported death of a full-time Latter-day Saint missionary this year
The first was a 26-year-old missionary from the Democratic Republic of Congo
who died March 10 in the hospital “a short time after he began feeling ill.” He had been serving in the Mbuji-Mayi Mission in his home country
The second was a 20-year-old missionary from Guatemala
who died April 11 while serving in the Honduras San Pedro Sula West Mission
She fell ill and was admitted to a hospital
“Doctors began emergency treatment,” the Utah-based church said
The third was a 19-year-old missionary from Canada, who was serving in the Utah Layton Mission when he suffered a traumatic brain injury and died in a Salt Lake City hospital May 8.
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