Literature DB >> 33855137

Dataset of pharmaceuticals and personal care products in a Mediterranean coastal wetland.

Daniele Sadutto1, Vicente Andreu1, Timo Ilo2, Jarkko Akkanen2, Yolanda Picó1.   

Abstract

The dataset provides information on Pharmaceutical and Personal Care Products (PPCPs) detected in the Albufera Natural Park (Valencia, Spain), a typical Mediterranean coastal wetland. These PPCPs constitute an important group of organic pollutants highly representative of the human impact. The concentrations values measured in soil, sediment and water and the statistical relationship of contaminants between them and with the environmental parameters could help to understand their fate in different compartments. The data also reported the occurrence and removal efficiency (%) for each contaminant in ten wastewater treatment plants (WWTPs), located in the surrounding area. This dataset could provide an idea on the effectiveness of WWTP treatments and the capacity of released PPCPs to affect the ecosystem. The extraction of analytes was based on solid-phase extraction (SPE) for water and solvent extraction followed by the previous SPE as clean-up for soil and sediment. Determination was carried out by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) with a triple-quadrupole. The present dataset was analyzed within the article entitled: "Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment"[1].
© 2021 The Author(s).

Entities:  

Keywords:  Albufera natural park; PPCPs; Sediment; Soil; Wastewater; Water

Year:  2021        PMID： 33855137      PMCID： PMC8027530          DOI： 10.1016/j.dib.2021.106934

Source DB:  PubMed          Journal:  Data Brief        ISSN： 2352-3409


Specifications Table

Value of the Data

The contaminants monitoring of a Natural Park (Albufera) is needed to value the environmental risk and how it is related with anthropogenic pressures. In addition, statistical correlations show a relationship between studied PPCPs and the different matrices. National and international authorities, wastewater treatment plant managers and researchers can estimate removal, occurrence, transport and fate of PPCPs. The data of PPCPs occurrence in sediment, soil and water samples could serve as a knowledge base that allows the establishment of monitoring programs for the compounds that appear with a higher frequency and establish a better assessment of the risks that exist for this natural space. The concentrations on each sampling point may help to understand the geophysical distribution of these contaminants and can be compared with other studies.

Data Description

The presented data were collected in the Albufera Natural Park (Valencia, Spain), which is included in the list of international wetlands (RAMSAR) (since 1990), in the Natura 2000 network as a Special Protection Area for Birds (SPA) under the Birds Directive, and is considered a Site of Community Importance (SCI) under Habitats Directive. This area of about 21000 hectares (ha) included a coastal lagoon fed by streams, rivers and irrigation channels, a sandy shoreline belt, rice paddies, vegetables and orange orchards in its most external part, where 43 sampling points and ten wastewater treatment plants (WWTPs), that discharged into irrigation channels that eventually end up in the park, were monitored. Strong anthropic pressure has already been noted in the area due to the proximity of Valencia city and its metropolitan area [3]. The occurrence of 32 pharmaceutical and personal care products (PPCPs) was investigated from November 2016 to February 2017. Detailed information of each sampling site is provided in the related article. Tables 1–2 shows the concentration of PPCPs in influent (i) and effluent (e) wastewater samples with relative date of collection. While, the removal efficiency (%) for each compound was reported in Table 3. The occurrence of (32) water, (19) sediment and (33) soil samples was described in Tables 4–6. The data presented in Table 1, Table 2 and 4–6 are the average value of three method's replicates for each sample to check reproducibility. In the public repository (Mendeley Data) [4] have been published the additional tables (named table S. “n°”), that contain the results of each individual extraction as well as the average (Tables S1-S5) and the linearity (R2), LOD, LOQ and matrix effect (ME) for each contaminant (Table S6-S7). The Statistical correlations between the studied PPCPs in soils, sediment and water were described in Tables 7–9. At last, statistical correlations between contaminants and intrinsic characteristics of all matrices were schematized in Tables 10–12. The intrinsic characteristics considered were temperature, pH, total soluble salts, dissolved O2 and redox potential in water, organic matter, carbonates, lime, clay and sand, pH, electric conductivity and cationic exchange capacity in sediments and organic matter, carbonates, sodium, potassium, magnesium and calcium, pH, electric conductivity and cationic exchange capacity in soil.
Table 1

Concentration of PPCPs (ng L−1) in the influents (i) of the WWTPs*.

CompoundiASiCATiCATiPALiSALiPEiPIiPIiPIIiPIIiPSiQBiSU
25/11/201622/11/201613/01/201714/12/201613/01/201713/01/201722/11/201613/01/201722/11/201613/01/201725/11/201614/12/201625/11/2016
Alprazolam2.30n.d.**2.424.031.433.013.824.344.234.012.337.121.91
Atenolol1325.6363.511322.916223633515424482.0257174
Atorvastatine83.12.6513415727.259.714827816623163.027461.0
Bezafibrate5.220.9152.31.621.213.0229.535.026.321.00.3231.03.12
BPA56237.14.27 × 10314766.287.91662384003871101.01 × 10392.0
Butylparaben5.43n.d.18.419.21.82n.d.13.633.01.9210.89.144.626.73
Caffeine8.70 × 1039.78 × 1039.36 × 1036.08 × 1032.46 × 1035.24 × 1039.99 × 1031.32 × 1036.95 × 1038.36 × 1034.34 × 10318.07 × 1034.3 × 103
Chloramphenicol2.01n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.41
Clofibric acidn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Codeine68.41.1252.27.0110.050.252.113380.993.847.571.872.0
Diclofenac324n.d.29030368.0123324380386320327348275
Enelapril379n.d.28363.8n.d.n.d.288281243141119510127
Ethylparaben25.04.3417487.25.323.0387.243.00.521.715.2143.073.0
Etoricoxib9.311.3217.414.86.036.9414.915.018.522.012.036.17.42
Flufenamic acid1260.8478.075.226.486.713617517820548.941595.3
Furosemide411n.d.354198n.d.268444700557598266927310
Ibuprofen11.0 × 1032.32 × 10312.60 × 1036.51 × 1032.57 × 1036.99 × 1037.97 × 1031.42 × 1037.79 × 10310.3 × 1035.58 × 10311.5 × 10357.6 × 103
Indomethacin6.03n.d.0.62n.d.1.03n.d.4.527.32n.d.3.82n.d.n.d.0.72
Lorazepam30.633.026.018.117.029.430.251.043.135.313.792.030.0
Metformin1903.6233832347.9286256410260321206319135
Methylparaben35424.238862559.01322861.28 × 10336.524.8164115610
Naproxen2.56 × 10350.43.58 × 1036325701.84 × 1032.85 × 1033.38 × 1032.55 × 1032.85 × 1032.10 × 1033.02 × 1032.00 × 103
Omeprazolen.d.n.d.1.0n.d.n.d.n.d.n.d.270n.d.n.d.n.d.n.d.158
Paracetamol2.83 × 1034.94 × 1035.92 × 1036.08 × 1033.15 × 1034.52 × 1034.34 × 1036.78 × 1031.86 × 1033.81 × 1035.50 × 1034.50 × 1035.35 × 103
Propylparaben18811.739528839.9319373627111224290134275
Salicylic acid7791672.01 × 1031.61 × 1032503941.41 × 1032.58 × 1032371877301.49 × 1031.76 × 103
Simvastatin2.06 × 103n.d.1.67 × 1031.30 × 1031866061.28 × 1032.02 × 1031.31 × 1032.03 × 1031.60 × 1032.05 × 1031.75 × 103
Thiamphenicoln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Tramadol5691535512971384195878596817502201.05 × 103416
Triclocarban0.740.42n.d.0.41n.d.0.531.721.511.120.630.910.820.71
Triclosan10240.499.577.050.0n.d.30841056.2133156153104
Warfarinn.d.n.d.0.330.54n.d.0.45n.d.n.d.1.15n.d.n.d.0.21n.d.

* WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS)

** n.d. = not detected

Table 2

Concentration of PPCPs (ng L−1) in the effluents (e) of the WWTPs*.

CompoundeASeCATeCATePALeSALePEePIePIePIIePIIePSeQBeSU
25/11/201622/11/201613/01/201714/12/201613/01/201713/01/201722/11/201613/01/201722/11/201613/01/201725/11/201614/12/201625/11/2016
Alprazolam3.20n.d.**n.d.5.901.602.307.505.109.007.002.907.704.60
Atenolol14.08.4014026.019.04.0014819012513711.710424.4
Atorvastatinen.d.n.d.n.d.n.d.n.d.n.d.15214352.9146n.d.19.015.7
Bezafibrate1.800.500.300.402.001.0029.635.16.9020.40.5020.412.3
BPA93.019.0n.d.35.811.041.018116565.324071.022183.0
Butylparaben0.40n.d.n.d.n.d.n.d.n.d.0.200.20n.d.1.50n.d.n.d.n.d.
Caffeine8.805.5043.014928.936.015.372.040.415126.845540.0
Chloramphenicoln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Clofibric acidn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Codeine14.11.400.207.103.507.3050.176.153.696.724.532.831.0
Diclofenac164n.d.n.d.16429.057.0711433525490114259199
Enelapriln.d.n.d.n.d.n.d.n.d.n.d.n.d.83.0n.d.n.d.n.d.n.d.n.d.
Ethylparabenn.d.n.d.0.200.300.500.40n.d.0.50n.d.1.000.604.000.30
Etoricoxib8.002.601.4019.53.704.7025.724.730.222.513.422.127.7
Flufenamic acid1370.40n.d.95.822.065.035020027720045.0328187
Furosemide134n.d.n.d.n.d.2.0030.090455055263066.1427313
Ibuprofenn.d.499231n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Indomethacinn.d.n.d.n.d.n.d.n.d.n.d.n.d.1.80n.d.7.90n.d.n.d.n.d.
Lorazepam18.1n.d.n.d.42.98.6017.061.354.463.157.128.046.636.5
Metformin6.502.004.409.901.108.0066.334.918.924.015.623.426.5
Methylparaben20.6n.d.n.d.13.65.604.6029.140.020.235.016.930.128.7
Naproxen23.0n.d.n.d.26.3n.d.n.d.75.4n.d.90.714626.1318205
Omeprazolen.d.n.d.n.d.n.d.n.d.n.d.30.014.025.623.04.0016.0n.d.
Paracetamol11.32.0019.034.849.039.018.137.016.615.424.137.070.0
Propylparaben1.30n.d.1.705.304.105.005.8010.03.708.703.006.202.30
Salicylic acid1.4058.4108380310248207345205325124580212
Simvastatinn.d.24580.0n.d.n.d.n.d.n.d.35.0n.d.n.d.n.d.n.d.n.d.
Thiamphenicoln.d.n.d.n.d.n.d.n.d.n.d.n.d.9.00n.d.14.8n.d.n.d.n.d.
Tramadol470n.d.3.505761204671.10 × 1039941.28 × 1031.30 × 10327311.6 × 103666
Triclocarbann.d.0.40n.d.0.300.100.100.600.50n.d.0.41.200.400.50
Triclosan24.0n.d.n.d.22.64.30n.d.29.220.310.47.4n.d.14.026.3
Warfarin0.50n.d.n.d.0.30n.d.n.d.n.d.n.d.0.800.7n.d.0.100.40

** WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS)

** n.d. = not detected

Table 3

Removal efficiency (%) for each PPCPs in each WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS).

CompoundASCATCATPALEPEPIPIPIIPIIPSEQBSALSU
25/11/201622/11/201613/01/201714/12/201613/01/201722/11/201613/01/201722/11/201613/01/201725/11/201614/12/201613/01/201725/11/2016
Alprazolam−37/*100−4722−99−18−115−75−26−9−12−146
Atenolol89−51−12077983743194486601786
Atorvastatine100100100100100−34968371009310074
Bezafibrate6651997266//743−6734−57−291
BPA83491007653−931843835788310
Butylparaben93/100100/989910086100100100100
Caffeine100100100989910099999899979999
Chloramphenicol100///////////100
Clofibric acid/////////////
Codeine79−26100−18544334−348546557
Diclofenac49/1004654−119−14−36−5365265728
Enelapril100/100100/10070100100100100/100
Ethylparaben100100100100871009910042899190100
Etoricoxib14−10892−3132−72−65−63−2−123939−275
Flufenamic acid−848100−2725−158−14−56282117−96
Furosemide67/10010089−103211−57554!−1
Ibuprofen1007998100100100100100100100100100100
Indomethacin100/100//10076/−108//100100
Lorazepam41100100−13742−103−7−46−62−1044949−22
Metformin97449997977491939392939880
Methylparaben941001009896909745−4190749095
Naproxen9910010096100971009695998910090
Omeprazole//100//!**95!!!!/100
Paracetamol10010010099991009999100100999899
Propylparaben9910010098989898979699959099
Salicylic acid8265957637858714−748361−2488
Simvastatin100!9510010010098100100100100100100
Thiamphenicol//////!/!////
Tramadol1710099−94−11−89−16−88−74−24−1013−60
Triclocarban10013/2985686710038−3149!26
Triclosan7610010071/91958294100919175
Warfarin!/10039100//26!/71/!

* “/” means that compound was not detected in influent and effluent wastewater samples **“!” means that compound was detected only in effluent wastewater sample.

Table 4

Concentration of PPCPs (ng L−1) in water samples (W.n°) of the Albufera Natural Park, Valencia, Spain.

CompoundW.1W.4W.5W.6W.7W.10W.11W.12W.14W.15W.16W.17W.18W.19W.20W.21W.22W.23W.26W.27W.29W.30W.31W.32W.33W.34W.36W.37W.38W.39W.40W.41W.42
Alprazolam10.04.00n.d.*6.00n.d.n.d.n.d.1.00n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.2.00n.d.8.00n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Atenolol320114n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.62.0n.d.n.d.n.d.n.d.n.d.n.d.78n.d.n.d.n.d.92.052.022172.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Atorvastatin1.00n.d.n.d.1.00n.d.n.d.n.d.n.d.21.0n.d.n.d.n.d.n.d.1.00n.d.n.d.n.d.n.d.n.d.n.d.2.001.00n.d.21.01.0021.01.0021.0n.d.1.0021.01.00n.d.
Bezafibrate79.063.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.00n.d.2.00n.d.n.d.n.d.9.00n.d.75.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Bisphenol A18514515012048.065.075.056.070.025.051.048.072.045.014057.031.012.019.011514019011515860.020519754.015015813081.0150
Butylparabenn.d.n.d.70.070.045.0n.d.n.d.n.d.n.d.40.0n.d.n.d.40.045.0n.d.40.0n.d.n.d.n.d.70.0n.d.n.d.70.0n.d.40.0n.d.71.0n.d.70.070.042.042.0n.d.
Caffeine15228.062.022.013756.011.014.029176.015221.013410112121940.066820.043.013854110327215766.017393.014112712016.018.0
Chloramphenicoln.d.n.d.n.d.50.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.39.040.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.40.0n.d.50.0n.d.n.d.50.0n.d.n.d.n.d.
Clofibric acid76.077.076.076.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.77.0n.d.n.d.n.d.n.d.77.076.075.076.076.0n.d.75.076.0n.d.76.076.075.0n.d.80.0
Codeine15427.0n.d.26.0n.d.n.d.n.d.n.d.n.d.n.d.8.00n.d.n.d.n.d.7.0016.0n.d.21.0n.d.n.d.n.d.36.030.084.012.0n.d.39.0n.d.n.d.n.d.n.d.n.d.n.d.
Diclofenac16970.050.011560.052.075.055.0n.d.75.090.067.072.063.0n.d.75.065.010375.0n.d.45.095.065.082.078.066.0n.d.10445.035.072.035.030.0
Enalapriln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.4.00n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.8.00n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Ethylparabenn.d.n.d.72.073.078.072.0n.d.82.0n.d.70.0n.d.70.070.070.0n.d.n.d.n.d.77.073.067.0n.d.75.066.067.080.079.070.076.065.0n.d.75.070.0n.d.
Etoricoxib18.04.003.008.001.00n.d.1.001.00n.d.n.d.2.00n.d.n.d.1.002.002.00n.d.2.00n.d.2.002.005.005.0013.0n.d.n.d.6.007.0025.020.03.003.005.00
Flufenamic Acid19585.060.0150n.d.1.00n.d.n.d.1.002.004.002.00n.d.n.d.61.07.001.0015.0n.d.n.d.n.d.80.080.014010.0n.d.n.d.1.00n.d.n.d.n.d.n.d.n.d.
Furosemiden.d.115n.d.74.048.0n.d.n.d.n.d.n.d.70.090.0n.d.n.d.n.d.n.d.n.d.n.d.65.0n.d.n.d.n.d.95.085.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Ibuprofen90.085.020.035.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.14460.0217n.d.n.d.n.d.90.0n.d.n.d.43.0n.d.n.d.n.d.
Indomethacin56.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.25.0n.d.n.d.n.d.24.0n.d.n.d.n.d.n.d.n.d.n.d.50.0n.d.25.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Lorazepam88.015.0n.d.15.0n.d.n.d.n.d.n.d.n.d.n.d.18.0n.d.n.d.n.d.n.d.6.00n.d.31.0n.d.n.d.n.d.23.012.070.01.00n.d.n.d.2.00n.d.n.d.n.d.5.00n.d.
Metformin25166.0n.d.19.020.04.003.005.0023.015.011426.01713.0014.055.02.0013137524.025.018670.093.057.018.022.033.094.040.040.06.0019.0
Methylparaben75.075.010773.082.074.075.080.077.075.079.072.075.074.0n.d.75.0n.d.82.075.0n.d.70.084.075.078.075.073.078.076.073.0n.d.75.082.074.0
Naproxen195145n.d.105n.d.n.d.n.d.n.d.115n.d.n.d.n.d.n.d.n.d.n.d.117114208111n.d.n.d.209225178160n.d.86.0n.d.n.d.n.d.113115n.d.
Omeprazolen.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Paracetamol26.0n.d.5.00n.d.32.014.011.017.082.028.018.0n.d.32.031.011.040.0n.d.168n.d.25.033.075.017.037.049.043.047.023.023.025.015.023.026.0
Propylparabenn.d.88.075.0n.d.38.033.032.035.033.032.030.030.030.030.075.035.030.033.030.090.075.075.075.013531.0n.d.75.031.075.070.032.0n.d.90.0
Salicylic Acid99.088.075.0113690602n.d.n.d.840282249n.d.29839129423920875134010652171375.0161230686166592240858386301204
Simvastatinn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Thiamphenicol35.0n.d.n.d.n.d.n.d.5.00n.d.1.00n.d.n.d.5.00n.d.n.d.n.d.n.d.n.d.n.d.5.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.5.0035.0
Tramadol12.6 × 1021971.00523n.d.11.013.012.03.005.0018.09.0033.07.007.084.0n.d.106n.d.22.027.033317169589.03.0050.024.056.042.018.0n.d.5.00
Triclocarbann.d.15.013.0n.d.n.d.2.00n.d.1.001.001.001.001.001.00n.d.n.d.5.00n.d.1.00n.d.14.0n.d.1.0013.0n.d.n.d.n.d.n.d.1.0013.013.015.01.0015.0
Triclosan65.028.0n.d.n.d.n.d.n.d.44.050.060.065.0n.d.51.055.048.015.072.0n.d.52.044.0n.d.25.0n.d.52.056.050.048.050.0n.d.45.031.035.065.020.0
Warfarin65.065.065.064.0n.d.45.0n.d.n.d.n.d.n.d.45.0n.d.48.0n.d.65.045.0n.d.n.d.45.0n.d.n.d.65.070.070.045.065.0n.d.46.065.065.0n.d.46.0n.d.

* n.d. = not detected

Table 6

Concentration of PPCPs (ng g−1) in soil samples (So.n°) of the Albufera Natural Park, Valencia, Spain.

CompoundSo.1So.2So.3So.4So.5So.6So.7So.8So.9So.10So.11So.12So.13So.14So.15So.16So.17So.20So.23So.24So.25So.26So.29So.30So.31So.32So.33So.34So.35So.41So.42So.43So.44
Alprazolamn.d.*67n.d.67n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Atenololn.d.n.d.n.d.n.d.n.d.n.d.n.d.2.01.0n.d.211.021n.d.1.021n.d.1.0211.0n.d.n.d.1.0n.d.n.d.n.d.n.d.21n.d.n.d.n.d.n.d.1.0
Atorvastatinn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Bezafibraten.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Bisphenol A9.06.03.09.0104.08.04.07.06.0104.03.04.02.03.02.03.01.02.02.07.02.09.04.0n.d.3.0158.09.0117.09.0
Butylparabenn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Caffeinen.d.22244.01.024n.d.3.024n.d.223.02.0231.0221.0223.01.0262323n.d.231.0233.0221613n.d.2.0
Chloramphenicol1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Clofibric Acidn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Codeinen.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.7.0n.d.n.d.n.d.n.d.n.d.7.0
Diclofenac2.03.01.01.0n.d.1.01.02.01.0n.d.n.d.n.d.n.d.n.d.n.d.2.0n.d.2.0n.d.n.d.n.d.n.d.n.d.n.d.3.0n.d.2.02.0n.d.n.d.2.01.0n.d.
Enalapriln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Ethylparaben3.0n.d.n.d.n.d.2.0n.d.n.d.3.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.3.0n.d.n.d.2.0n.d.n.d.n.d.n.d.n.d.3.0n.d.
Etoricoxibn.d.n.d.n.d.1.0n.d.n.d.51n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Flufenamic Acid1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Furosemiden.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Ibuprofen2.04.010n.d.7.04.03.0n.d.3.0n.d.n.d.n.d.3.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.7.0n.d.n.d.n.d.n.d.8.0n.d.4.0n.d.763.0n.d.
Indomethacinn.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Lorazepamn.d.n.d.62n.d.n.d.n.d.n.d.n.d.n.d.n.d.62n.d.n.d.62n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Metforminn.d.n.d.n.d.4747n.d.1.0n.d.n.d.n.d.n.d.47n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.48n.d.n.d.n.d.n.d.n.d.n.d.n.d.47n.d.
Methylparabenn.d.3.02.02.02.03.03.02.02.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.4.0n.d.n.d.2.0n.d.n.d.2.02.02.0n.d.n.d.
Naproxen1.0n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.1.01.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.
Omeprazolen.d.n.d.n.d.2.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.4.0n.d.4.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.3.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Paracetamoln.d.n.d.30n.d.n.d.1.0n.d.n.d.30n.d.n.d.n.d.n.d.n.d.n.d.303031n.d.n.d.30n.d.n.d.n.d.n.d.30n.d.n.d.31n.d.n.d.n.d.n.d.
Propylparabenn.d.n.d.n.d.n.d.n.d.n.d.2.0n.d.2.0n.d.n.d.1.0n.d.n.d.1.01.0n.d.n.d.n.d.3.0n.d.2122n.d.3.0n.d.n.d.3.02.02.0114.0n.d.
Salicylic Acid9.0n.d.n.d.n.d.2.0n.d.n.d.n.d.3.0n.d.2.02.0202.06.0n.d.5.0n.d.2.01.0n.d.n.d.n.d.3.0n.d.n.d.n.d.6.018n.d.n.d.n.d.5.0
Simvastatinn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.
Thiamphenicoln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.3.0
Tramadoln.d.n.d.n.d.2.0n.d.1.060n.d.60n.d.n.d.n.d.n.d.n.d.60n.d.60n.d.n.d.n.d.n.d.n.d.n.d.60n.d.1.0n.d.n.d.n.d.n.d.60n.d.60
Triclocarban1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.2.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Triclosan4.03.0n.d.n.d.n.d.1.0n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.4.0n.d.n.d.1.0n.d.1.0n.d.n.d.n.d.n.d.n.d.5.0n.d.n.d.n.d.
Warfarin1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.

* n.d. = not detected

Table 7

Statistical correlations between the studied pharmaceuticals in soils (** Significant correlation at level of P= 0.01. * Significant correlation at level of P= 0.05).

AtenAtorvBZFBisABPNCafCPLCodDFCEtorEPBFlufAIbupIMTNLZMMetMPNNapOPZPmolPPNSalASVTNTPLTramTCBNTCSN
Aten
Atorv.592⁎⁎
BZF
BisA
BPN.417*.448⁎⁎
Caf
CPL.726⁎⁎
Cod
DFC
Etor
EPB.391*
FlufA.641⁎⁎.915⁎⁎
Ibup
IMTN
LZM.352*
Met−.395*
MPN
Nap.437*.506⁎⁎
OPZ
Pmol−.352*.349*
PPN
SalA.375*
SVTN.382*
TPL.697⁎⁎
Tram
TCBN.382*.420*
TCSN.419*.436*.482⁎⁎
War.646⁎⁎.940⁎⁎.446⁎⁎.878⁎⁎.429*.369*

Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. ClorA: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. FlufA: Flufenamic Acid. Ibup: Ibuprofen. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. MPN: Methylparaben. Nap: Naproxen. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin.

Table 9

Statistical correlations between the studied pharmaceuticals in waters (** Significant correlation at level of P= 0.01, * Significant correlation at level of P= 0.05).

AlprazAtenAtorvBZFBisABPNCafCPLClorACodDFCEtorEPBFlufAFuroIbupIMTNLZMMetMPNNapPmolPPNTPLTram
Aten.830⁎⁎
Atorv
BZF.858⁎⁎.899⁎⁎
BisA.383*.374*
BPN
CPL.526⁎⁎
ClorA.906⁎⁎
Cod.871⁎⁎.929⁎⁎.830⁎⁎.423*.358*
DFC.584⁎⁎.598⁎⁎.442⁎⁎.550⁎⁎
Etor.469⁎⁎.410*.410*.532⁎⁎.538⁎⁎.472⁎⁎
FlufA.908⁎⁎.773⁎⁎.745⁎⁎.454⁎⁎.503⁎⁎.828⁎⁎.530⁎⁎.416*
Ibup.422*.498⁎⁎.372*.393*.368*
IMTN.356*.521⁎⁎.589⁎⁎.421*.450⁎⁎.510⁎⁎
LZM.870⁎⁎.956⁎⁎.848⁎⁎.380*.935⁎⁎.624⁎⁎.445⁎⁎.803⁎⁎.456⁎⁎
Met.477⁎⁎.439*.476⁎⁎.461⁎⁎
MPN.376*.377*
Nap.462⁎⁎.609⁎⁎.463⁎⁎.528⁎⁎.593⁎⁎.401*.550⁎⁎.370*.395*.466⁎⁎.586⁎⁎.435*
Pmol.874⁎⁎.345*
PPN.427*.554⁎⁎−.418*
SalA.354*.513⁎⁎.572⁎⁎
TPL.406*.475⁎⁎.372*.510⁎⁎.377*.475⁎⁎
Tram.951⁎⁎.890⁎⁎.808⁎⁎.401*.371*.953⁎⁎.641⁎⁎.514⁎⁎.899⁎⁎.534⁎⁎.924⁎⁎.423*.546⁎⁎.494⁎⁎
TCBN.435*.535⁎⁎.480⁎⁎
TCSN.387*
War.412*.386*.374*.448⁎⁎.401*.362*.473⁎⁎.570⁎⁎.364*.419*

Aten: Atenolol. Alpraz: Alprazolam. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. CPL: Chloramphenicol. ClorA: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. FlufA: Flufenamic Acid. Ibup: Ibuprofen. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. MPN: Methylparaben. Nap: Naproxen. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin.

Table 10

Statistical correlations between pharmaceuticals and intrinsic soil characteristics (** Significant correlation at level of P = 0.01. * Significant correlation at level of P = 0.05).

pHECCO3OMNaKMgCaCEC
Alpraz−.380*.410*.451⁎⁎
BisA.358*.421*.372*
Ibup.353*
MPN−.376*.444⁎⁎
Nap−.364*
PPN−.352*
TPL.354*.446⁎⁎
TCSN.359*
War.396*.414*

EC: Electric conductivity. CO: Carbonates. OM: Organic Matter. Na: Sodium. K: Potasium. Mg: Magnesium. Ca: Calcium. CEC: Cation Exchange Capacity.

Alpraz: Alprazolam. BisA: Bisphenol A. Ibup: Ibuprofen. MPN: Methylparaben. Nap: Naproxen. PPN: Propylparaben. TPL: Thiamphenicol. TCSN: Triclosan. War: Warfarin.

Table 12

Statistical correlations between the studied pharmaceuticals and intrinsic characteristics of waters (** Significant correlation at level of P = 0.01, * Significant correlation at level of P = 0.05).

pHTECTDSRestNaClDO%Cl−NO2−NO3=SO4=NaKMgCa
Alpraz−.446⁎⁎
Aten−.414*
Atorv.354*
BisA
Caf−.410*−.365*−.388*−.385*
ClorA−.355*−.345*−.393*−.361*
Cod−.458⁎⁎
Enal.721⁎⁎
EPB.371*
FlufA−.398*
Furo−.361*.381*−.377*
IMTN.473⁎⁎
LZM−.477⁎⁎
Met.694⁎⁎
Nap.359*.387*−.480⁎⁎
Pmol−.354*−.356*
SalA−.402*−.387*−.373*
TPL−.420*.364*.736⁎⁎
Tram−.491⁎⁎
TCBN.440*−.355*

T: temperature (°C). EC: Electric Conductivity (dS/m). TDS: Total Dissolved Solids (mg/L). Rest: Resistivity (Ώ). DO%: Dissolved Oxygen (%). Cl: Chlorides (mg/L). NO: Nitrites. NO: Nitrates (mg/L). SO: Sulfates (mg/L). Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. Caf: Caffeine. ClorA: Clofibric Acid. Cod: Codeine. EPB: Ethylparaben. FlufA: Flufenamic Acid. Furo: Furosemide. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. Nap: Naproxen. Pmol: Paracetamol. SalA: Salicylic Acid. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban.

Concentration of PPCPs (ng L−1) in the influents (i) of the WWTPs*. * WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS) ** n.d. = not detected Concentration of PPCPs (ng L−1) in the effluents (e) of the WWTPs*. ** WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS) ** n.d. = not detected Removal efficiency (%) for each PPCPs in each WWTPs: Pinedo 1 (PI), Pinedo 2 (PII), Port de Catarroja (CAT), Quart - Benàger (QB), Sueca (SU), Perelló-Sueca (PS), Perellonet (PE), Palmar (PAL), Saler (SAL) and Albufera Sud (AS). * “/” means that compound was not detected in influent and effluent wastewater samples **“!” means that compound was detected only in effluent wastewater sample. Concentration of PPCPs (ng L−1) in water samples (W.n°) of the Albufera Natural Park, Valencia, Spain. * n.d. = not detected Concentration of PPCPs (ng g−1) in sediment samples (S.n°) of the Albufera Natural Park, Valencia, Spain. * n.d. = not detected Concentration of PPCPs (ng g−1) in soil samples (So.n°) of the Albufera Natural Park, Valencia, Spain. * n.d. = not detected Statistical correlations between the studied pharmaceuticals in soils (** Significant correlation at level of P= 0.01. * Significant correlation at level of P= 0.05). Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. ClorA: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. FlufA: Flufenamic Acid. Ibup: Ibuprofen. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. MPN: Methylparaben. Nap: Naproxen. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin. Statistical correlations between pharmaceuticals in sediments (** Significant correlation at level of P= 0.01, * Significant correlation at level of P= 0.05). Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. Clor A: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. Fluf A: Flufenamic Acid. Furo: Furosemide. Ibup: Ibuprofen. Met: Metformin. MPN: Methylparaben. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin. Statistical correlations between the studied pharmaceuticals in waters (** Significant correlation at level of P= 0.01, * Significant correlation at level of P= 0.05). Aten: Atenolol. Alpraz: Alprazolam. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. CPL: Chloramphenicol. ClorA: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. FlufA: Flufenamic Acid. Ibup: Ibuprofen. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. MPN: Methylparaben. Nap: Naproxen. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin. Statistical correlations between pharmaceuticals and intrinsic soil characteristics (** Significant correlation at level of P = 0.01. * Significant correlation at level of P = 0.05). EC: Electric conductivity. CO: Carbonates. OM: Organic Matter. Na: Sodium. K: Potasium. Mg: Magnesium. Ca: Calcium. CEC: Cation Exchange Capacity. Alpraz: Alprazolam. BisA: Bisphenol A. Ibup: Ibuprofen. MPN: Methylparaben. Nap: Naproxen. PPN: Propylparaben. TPL: Thiamphenicol. TCSN: Triclosan. War: Warfarin. Statistical correlations between pharmaceuticals and intrinsic sediment characteristics (** Significant correlation at level of P = 0.01, * Significant correlation at level of P = 0.05). OM: Organic Matter. CO: Carbonates. Sac: Lime + clay fractions. SandT: Total sand fraction. EC: Electric conductivity. CEC: Cation Exchange Capacity. Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. Clor A: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. Fluf A: Flufenamic Acid. Furo: Furosemide. Ibup: Ibuprofen. Met: Metformin. MPN: Methylparaben. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCSN: Triclosan. War: Warfarin. Statistical correlations between the studied pharmaceuticals and intrinsic characteristics of waters (** Significant correlation at level of P = 0.01, * Significant correlation at level of P = 0.05). T: temperature (°C). EC: Electric Conductivity (dS/m). TDS: Total Dissolved Solids (mg/L). Rest: Resistivity (Ώ). DO%: Dissolved Oxygen (%). Cl: Chlorides (mg/L). NO: Nitrites. NO: Nitrates (mg/L). SO: Sulfates (mg/L). Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. Caf: Caffeine. ClorA: Clofibric Acid. Cod: Codeine. EPB: Ethylparaben. FlufA: Flufenamic Acid. Furo: Furosemide. IMTN: Indomethacin. LZM: Lorazepam. Met: Metformin. Nap: Naproxen. Pmol: Paracetamol. SalA: Salicylic Acid. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban.

Experimental Design, Materials and Methods

The water characteristics were in situ measured using a portable Multiparameter Eutech Instrument CyberScan PCD 650 (Thermo Fisher Scientific, Basel, Switzerland). The soil and sediment characteristics were established in the laboratory using standard procedures. Organic matter was determined by oxidation with dichromate [5]. Carbonate was determined using the Bernard calcimeter [6] method and cationic exchanger capacity was calculated measuring sodium, potassium, magnesium and calcium by extraction with 1 M ammonium acetate solution and inductively coupled plasma optical emission spectroscopy) (ICP-OES) following the method of Rhoades [7]. Electric conductivity and pH were determined in the soil saturation extract with a pH-meter according to Richards [8] and finally, % of lime, clay and sand were established using an hydrometer according to the Bouyoucos [9] method. The waste and surface waters (200 mL) were vacuum filtered by a 0.6-µm glass fiber filter (GA-55, 90 mm - Advantec MFS, Dublin, CA, USA) and stored at -20°C until the analysis. The sediments were lyophilized with a Virtis lyophilizer (SP Scientific, Gardiner, NY, USA) and the soil samples were sieved, and air-dried in the dark at 20°C to reduce the moisture content. The samples of water, soil and sediment were spiked with labeled internal standards to quantify the PPCPs present in the all environmental compartments. A previous solid-liquid extraction was performed for solid samples (1g), with the use of 15 mL of a mix containing Milli-Q water, McIlvaine–EDTA buffer and methanol (MeOH) in equal parts. The mixture was homogenized for 5 min by vortex agitation, sonicated for 10 min, and centrifuged for 6 min at 3000 rpm and 10°C. The supernatant was separated and diluted with Milli-Q water to 200 mL. Then, the dilution was treated such as water extraction procedure. The clean-up that involves PPCPs isolation and concentration were performed by Solid Phase Extraction (SPE). Two methods employing different cartridges Strata-X and Strata-X-CW (Phenomenex, 33 µm, 200 mg/6 mL) characterized by a polymeric reversed and polymeric weak cation-exchange stationary phase, respectively, were used. Strata-X was activated with 6 mL MeOH, 6 mL Milli-Q water and with 6 mL 2mM Sodium Dodecyl Sulphate (SDS) solution (SDS method). While, Strata-X-CW was activated without SDS solution (WC method). The analytes were eluted with 6mL of MeOH and 3 mL of MeOH–DCM (50:50 v/v) for reversed phase and with 6 mL of MeOH–NH4OH (95:5 v/v) for weak cation-exchange phase by gravity. The eluates were evaporated at 40°C and redissolved to 1 mL with mobile phase before injection. Alprazolam, atorvastatin, caffeine, chloramphenicol, diclofenac, flufenamic acid, furosemide, ibuprofen, omeprazole, paracetamol and thiamphenicol were detected by WC method in water, sediment and soil matrix. While, atenolol, bezafibrate, butylparaben, clorfibric acid, enalapril, ethylparaben, etoricoxib, indomethacin, lorazepam, metformin, methylparaben, naproxen, propylparaben, salicylic acid, simvastatin tramadol, triclocarban, triclosan, warfarin by SDS method. Only bisphenol A and codeine were determined by both methods, SDS in water matrix and WC in sediment and soil. Instrumental analysis was performed by 1260 Infinity UHPLC (ultra-high-performance liquid chromatography) system coupled to mass spectrometry with a triple quadrupole mass detector (6410 QqQ-MS) from Agilent Technologies (Santa Clara, CA, USA). The electrospray ionization (ESI) was applied in negative and positive mode. The mobile phase consisted of MeOH (solvent A) and water (solvent B) both with NH4F at 2.5 mmol L−1 for negative mode and MeOH (solvent A) and water (solvent B) with 0.1% formic acid in both solutions for positive mode. The calibration curves used to quantify the environmental contaminants were prepared in H2O-MeOH (70-30) and in solvent with SDS to obtain correct quantification of those compounds. The qualitative and quantitative analysis of each chromatogram were performed by MassHunter Workstation (version 10.0 Software) supplied by Agilent Technologies. The statistical relationship of the different contaminants between them and with the environmental parameters in the three matrices selected (water, soil and sediment) was carried out by Statistical package IBM SPSS (version 26.0). The limits of detection (LODs) and limits of quantification (LOQs) were estimated experimentally, spiking blank samples, at the lowest concentration (10 ng g−1 and 50 µgL−1), with the PPCPs pre-extraction and estimating the analyte concentration able to provide a signal-to-noise ratio of 3 and 10 respectively. The LODs ranged from 1.65 and 16.65 ngL−1 in waste and surface water, and from 0.33 and 6.67 ng g−1 dry weight (d.w.) in sediment and soil. Particularly, to established the matrix effects (ME) two eight point calibration curves (10, 25, 50, 75, 100, 250, 500, 1000 ng/mL) were compared: (i) one prepared in solvent (that is H2O-MeOH (70-30) or this mixture with SDS depending on the method) and (ii) the other prepared in blank matrix extract, also redissolving the extract in H2O-MeOH (70-30) or this mixture with SDS. Then, the ME was calculated according to the formula: This information together with other experimental information were described in the Sadutto [2] work.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships, which have, or could be perceived to have, influenced the work reported in this article.
SubjectPollution
Specific subject areaPharmaceuticals and personal care products occurrence and fate in Mediterranean coastal wetlands.
Type of dataTable
How data were acquiredRaw data were acquired via HPLC-MS/MS. The instrument was an Infinity 1260 UHPLC system, coupled to mass spectrometry with a triple-quadrupole mass detector 6410 (QqQ-MS) from Agilent Technologies (Santa Clara, CA, USA). The ionization technique used was electrospray ionization (ESI).
Data formatRawAnalyzedFiltered
Parameters for data collectionThe mobile phase consisted of 2.5 mmol L−1 NH4F in methanol (A) and 2.5 mmol L−1 NH4F in water (B) for negative mode and methanol and water with 0.1% formic acid in both solutions for positive mode.The other parameters are described in literature [2].
Description of data collectionData were obtained analysing environmental samples (soil, sediment and water) collected in 44 sampling points of the Albufera Natural Park and in ten wastewater treatment plants (WWTPs), located in the surrounding area. The final value concentrations were achieved by HPLC-MS/MS analysis.
Data source locationInstitution: University of Valencia, Research Center on Desertification (CIDE)City: ValenciaCountry: SpainLatitude and longitude (and GPS coordinates, if possible) for collected samples/data: All coordinates are specified in related research article [1].Moreover, the virtual map of sampling points was reported in the interactive link:https://www.google.com/maps/d/viewer?mid=1ITmoW9a9uCVfqVZ08v25oNgMxjUFAMxn&ll=39.41350461328517%2C-0.41794440579224323&z=11
Data accessibilityPico, Yolanda; Sadutto, Daniele; Andreu, Vicente; Ilo, Timo; Akkanen, Jarkko (2021), “Details on the Dataset of pharmaceuticals and personal care products in a Mediterranean coastal wetland”, Mendeley Data, V1, http://dx.doi.org/10.17632/zy2zg7dhgv.1
Related research articleDaniele Sadutto, Vicente Andreu, Timo Ilo, Jarkko Akkanen, Yolanda Picó.Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment, Environmental Pollution, 2021, 271: p. 116353.https://doi.org/10.1016/j.envpol.2020.116353
Table 5

Concentration of PPCPs (ng g−1) in sediment samples (S.n°) of the Albufera Natural Park, Valencia, Spain.

CompoundS.5S.9S.10S.15S.16S.17S.18S.23S.26S.30S.33S.34S.35S.36S.37S.38S.39S.40S.41
Alprazolamn.d.*n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Atenololn.d.3.0n.d.n.d.2.05.04.04.03.05.05.03.01.0n.d.1.04.0n.d.n.d.16
Atorvastatinn.d.n.d.n.d.n.d.n.d.n.d.n.d.2.01.0n.d.211.021n.d.1.021n.d.1.021
Bezafibraten.d.n.d.n.d.3.0n.d.n.d.3.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.3.03.0n.d.
Bisphenol An.d.15205.0147.010217.02018202.0n.d.9.0141919n.d.
Butylparaben6.06.0n.d.6.07.0n.d.6.0n.d.n.d.6.06.0n.d.6.0n.d.6.06.06.06.0n.d.
Caffeine6.09.08.0107.05.08.08.06.07.06.09.06.04.05.04.06.0107.0
Chloramphenicoln.d.4.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Clofibric acidn.d.5.0n.d.n.d.n.d.n.d.5.05.05.0n.d.4.05.04.04.05.04.05.05.05.0
Codeinen.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Diclofenac3.03.08.08.0106.07.05.0n.d.3.06.06.06.0n.d.5.03.08.04.04.0
Enalapriln.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Ethylparabenn.d.1715n.d.16n.d.n.d.15151815171815n.d.15171518
Etoricoxib1.0n.d.1.0n.d.n.d.6.0n.d.1.01.01.01.01.0n.d.2.01.01.01.01.01.0
Flufenamic Acid2.02.02.02.02.02.02.02.02.03.02.02.02.02.02.02.02.02.02.0
Furosemide109.09.012142212229.0131548109.09.09.09.09.010.0
Ibuprofen471310 x 1012422303570227.0232963n.d.388.0n.d.284.0
Indomethacinn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Lorazepamn.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Metformin4.02.01.01.05.03.01.04.01.02.02.01.02.01.01.01.02.01.01.0
Methylparabenn.d.1313n.d.14n.d.13n.d.1718181819n.d.13n.d.1414n.d.
Naproxenn.d.n.d.n.d.2.0n.d.n.d.n.d.315.0n.d.8.0n.d.n.d.2.04.07.07.010.0n.d.
Omeprazolen.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.1.0n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.
Paracetamoln.d.6.0n.d.2.02.01.0n.d.n.d.33n.d.1.0n.d.n.d.2.0n.d.6.06.03.0n.d.
Propylparaben4.02.0n.d.2.0n.d.n.d.2.04.0n.d.2.09.09.09.09.0129.09.09.09.0
Salicylic Acid21182532282423231923182319191615182127
Simvastatin8.0212113n.d.2912n.d.n.d.17n.d.12n.d.n.d.n.d.18n.d.n.d.4.0
Thiamphenicol12n.d.119.0109.011111214n.d.1.0n.d.n.d.n.d.n.d.n.d.1.0n.d.
Tramadoln.d.n.d.1.0n.d.1.02.02.02.0n.d.132.0n.d.n.d.n.d.n.d.n.d.n.d.1.01.0
Triclocarbann.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.n.d.7915n.d.8.0105.05.012
Triclosan10148.07.08.08.013189.0178.09.08.08.08.08.09.08.08.0
Warfarin8.09.09.09.09.09.09.09.09.09.09.09.08.08.08.08.09.08.08.0

* n.d. = not detected

Table 8

Statistical correlations between pharmaceuticals in sediments (** Significant correlation at level of P= 0.01, * Significant correlation at level of P= 0.05).

AlprazAtenAtorvBZFBisABPNCafCPLClorACodDFCEtorEPBFlufAFuroIbupMetMPNOPZPmolPPNSalASVTNTPLTramTCBNTCSNWar
Alpraz−.377*
Aten
Atorv.454⁎⁎
BZF
BisA−.363*.363*
BPN.371*
Caf.522⁎⁎.375*
CPL
ClorA
Cod.459⁎⁎.750⁎⁎
DFC.365*.385*−.337*
Etor.349*−.516⁎⁎−.366*
EPB.347*.402*.329*
FlufA.453⁎⁎
Furo.334*.334*−.401*.408*
Ibup
Met−.416⁎⁎.363*
MPN.465⁎⁎−.332*.370*.330*
OPZ.375*.376*
Pmol−.458⁎⁎
PPN.469⁎⁎.638⁎⁎−.329*
SalA.325*.572⁎⁎−.561⁎⁎.515⁎⁎−.497⁎⁎
SVTN.373*.341*−.456⁎⁎.393*−.504⁎⁎
TPL−.497⁎⁎−.652⁎⁎−.354*−.330*.362*.454⁎⁎−.821⁎⁎.468⁎⁎
Tram.461⁎⁎−.357*.830⁎⁎.428⁎⁎
TCSN.482⁎⁎.374*.327*.644⁎⁎.350*.453⁎⁎.614⁎⁎−.409*
War−.377*.395*−.425⁎⁎.427⁎⁎.452⁎⁎.339*.545⁎⁎−.581⁎⁎.492⁎⁎−.581⁎⁎.497⁎⁎

Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. Clor A: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. Fluf A: Flufenamic Acid. Furo: Furosemide. Ibup: Ibuprofen. Met: Metformin. MPN: Methylparaben. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCBN: Triclocarban. TCSN: Triclosan. War: Warfarin.

Table 11

Statistical correlations between pharmaceuticals and intrinsic sediment characteristics (** Significant correlation at level of P = 0.01, * Significant correlation at level of P = 0.05).

OMCO3=SacSandTpHECCEC
Alpraz−.459⁎⁎
Aten
Atorv
BZF
BisA.408*
BPN.355*
Caf−.484⁎⁎.555⁎⁎−.325*
CPL
ClorA.348*.379*
Cod
DFC
Etor.384*
EPB
FlufA.378*−.398*
Furo−.382*
Ibup−.334*−.366*.345*−.335*
Met
MPN.426⁎⁎−.579⁎⁎−.399*
OPZ−.344*
Pmol.348*
PPN.512⁎⁎.477⁎⁎.565⁎⁎−.490⁎⁎.510⁎⁎.368*
SalA−.501⁎⁎−.614⁎⁎−.612⁎⁎.582⁎⁎
SVTN−.345*−.328*
TPL−.586⁎⁎−.470⁎⁎.406*−.401*
Tram
TCSN
War−.402*−.407*

OM: Organic Matter. CO: Carbonates. Sac: Lime + clay fractions. SandT: Total sand fraction. EC: Electric conductivity. CEC: Cation Exchange Capacity.

Alpraz: Alprazolam. Aten: Atenolol. Atorv: Atorvastatin. BZF: Bezafibrate. BisA: Bisphenol A. BPN: Butylparaben. Caf: Caffeine. CPL: Chloramphenicol. Clor A: Clofibric Acid. Cod: Codeine. DFC: Diclofenac. Etor: Etoricoxib. EPB: Ethylparaben. Fluf A: Flufenamic Acid. Furo: Furosemide. Ibup: Ibuprofen. Met: Metformin. MPN: Methylparaben. OPZ: Omeprazole. Pmol: Paracetamol. PPN: Propylparaben. SalA: Salicylic acid. SVTN: Simvastatin. TPL: Thiamphenicol. Tram: Tramadol. TCSN: Triclosan. War: Warfarin.

  3 in total

1.  Assessment of the occurrence and distribution of pharmaceuticals in a Mediterranean wetland (L'Albufera, Valencia, Spain) by LC-MS/MS.

Authors:  Pablo Vazquez-Roig; Vicente Andreu; Matthias Onghena; Cristina Blasco; Yolanda Picó
Journal:  Anal Bioanal Chem       Date:  2011-03-17       Impact factor: 4.142

2.  Systematic assessment of extraction of pharmaceuticals and personal care products in water and sediment followed by liquid chromatography-tandem mass spectrometry.

Authors:  Daniele Sadutto; Rodrigo Álvarez-Ruiz; Yolanda Picó
Journal:  Anal Bioanal Chem       Date:  2020-01-02       Impact factor: 4.142

3.  Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment.

Authors:  Daniele Sadutto; Vicente Andreu; Timo Ilo; Jarkko Akkanen; Yolanda Picó
Journal:  Environ Pollut       Date:  2020-12-22       Impact factor: 8.071
  3 in total

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