Supplementary material of the article “Survey regarding the occurrence of selected organic micropollutants in the groundwaters of overseas departments” (Environmental Science and Pollution Research, Vulliet et al.)
Corresponding author: Emmanuelle Vulliet,
Table S1
Retention time (Rt) during the analyses by LC-MS/MS, MRM transitions, linear range, limit of quantification (LOQ), declustering potential (DP) and collision energy voltages (CE) of two MRM transitions, recoveries, percentage of relative standard deviation (%RSD) and repeatability expressed as the %RSD.
Compounds / Rt(min) / MRM1; MRM2 / DP
(V) / CE
(eV) / Linear range (ng/L) / LOQ
(ng/L) / Recoveries (%RSD)
at 10xLOQ / % RSD
(at LOQ)
Positive ESI mode
Atenolol / 0.9 / 267.0→145.0; 267.0→74.0 / 81; 81 / 37; 31 / 0.4-28 / 1 / 86.3 (6.1) / 20.7
Acetaminophen / 1.3 / 151.8→110.2; 151.8→64.9 / 81; 81 / 21; 43 / 4-272 / 8 / 70.5 (18.9) / 21.3
Metronidazole / 1.4 / 171.9→128.0; 171.9→82.1 / 76; 76 / 21; 37 / 2-145 / 4 / 44.0 (24.7) / 20.4
Trimethoprim / 2.0 / 291.0→230.0; 291.0→261.0 / 136; 136 / 33; 37 / 0.5-29 / 1 / 105.9 (16.8) / 11.3
Norfloxacine / 2.2 / 320.0→302.0; 320.0→276.0 / 121; 121 / 29; 25 / 2-152 / 5 / 43.8 (22.7) / 18.8
Ofloxacine / 2.2 / 362.1→318.1; 362.1→261.0 / 111; 111 / 27; 37 / 2-47 / 4 / 67.2 (25.7) / 22.4
Methomyl / 2.3 / 163.0→88.0; 163.0→108.0 / 56; 56 / 15; 15 / 0.2-13 / 0.4 / 65.3 (22.6) / 19.4
Ciprofloxacine / 2.3 / 332.0→314.0; 332.0→231.0 / 91; 91 / 31; 51 / 3-70 / 6 / 55.8 (12.5) / 21.9
Caffeine / 2.5 / 195.0→138.0; 195.0→110.0 / 106; 106 / 27; 33 / 0.5-29 / 1 / 84.2 (18.7) / 21.9
Sulfamethasine / 2.6 / 279.0→186.0; 279.0→92.0 / 66; 66 / 25; 43 / 1-19 / 2 / 91.4 (6.3) / 22.3
Sulfamethoxazole / 2.7 / 253.9→156.0; 253.9→92.0 / 76; 76 / 23; 31 / 1-55 / 2 / 96.1 (8.5) / 14.6
Carbendazim / 2.3 / 192.0→160.0; 192.0→131.9 / 161; 161 / 29; 41 / 0.5-10 / 1 / 93.9 (7.8) / 14.2
Metoprolol / 2.6 / 268.0→77.0; 268.0→116.0 / 96; 96 / 77; 27 / 0.5-10 / 1 / 87.7 (7.0) / 13.6
Fluroxypyr / 4.0 / 255.0→209.0; 255.0→181.0 / 66; 66 / 21; 33 / 4-228 / 7 / 44.4 (32.7) / 6.9
Propranolol / 3.2 / 260.0→116.0; 260.0→56.0 / 101; 101 / 25; 45 / 4-262 / 8 / 73.9 (5.0) / 22.3
3,4-Dichloroaniline / 4.5 / 162.0→127.0; 162.0→74.0 / 121; 121 / 29; 65 / 9-580 / 17 / 39.4 (22.6) / 21.3
Carbofurane / 4.6 / 222.0→165.0; 222.0→123.0 / 76; 76 / 17; 31 / 0.4-9 / 1 / 47.4 (9.4) / 72.0
Carbamazepine / 5.3 / 236.9→193.9; 236.9→192.0 / 111; 111 / 27; 31 / 0.2-5 / 0.4 / 118.8 (5.9) / 6.2
Atrazine / 5.6 / 216.0→68.0; 216.0→68.0 / 76; 76 / 25; 51 / 0.4-9 / 1 / 104.7 (18.6) / 11.5
Diuron / 5.6 / 233.0→72.0; 233.0→159.9 / 111; 111 / 31; 35 / 1-30 / 3 / 100.7 (10.6) / 18.1
Isoproturon / 5.8 / 207.2→72.2; 207.2→165.4 / 60; 60 / 37; 17 / 0.4-28 / 1 / 97.7 (17.9) / 12.5
Oxazepam / 5.9 / 286.9→241.1; 286.9→269.0 / 121; 121 / 37; 21 / 2-140 / 4 / 79.4 (21.5) / 8.3
Matezachlor / 6.0 / 278.2→134.3; 278.2→210.3 / 60; 60 / 27; 15 / 0.2-15 / 0.4 / 85.6 (17.2) / 19.7
Lorazepam / 6.1 / 321.8→276.0; 321.8→304.0 / 116; 116 / 31; 21 / 4-284 / 9 / 75.5 (20.3) / 12.9
Tylosine / 6.4 / 916.4→174.1; 916.4→772.4 / 106; 106 / 49; 41 / 50-3000 / 100 / 98.2 (23.8) / 22.8
Clomazone / 6.4 / 240.1→125.1; 240.1→89.0 / 60; 60 / 23; 59 / 0.2-13 / 0.4 / 63.8 (31 / 14.4
Ketoprofen / 6.5 / 255.1→77.0; 255.1→209.1 / 101; 101 / 63; 19 / 1-58 / 2 / 91.8 (20.9) / 23.3
Bezafibrate / 6.9 / 362.0→138.9; 362.0→316.1 / 86; 86 / 33; 19 / 0.5-30 / 1 / 101.4 (20.5) / 10.6
Norethindrone / 7.0 / 299.0 →109.0; 299.0→77.0 / 131; 131 / 39; 87 / 1-85 / 3 / 102.3 (24.7) / 21.3
Androstenedione / 7.0 / 287.1→97.0; 287.1→109.1 / 126; 126 / 27; 29 / 0.4-28 / 1 / 8.2 (23.8) / 22.8
Azoxystrobin / 7.0 / 404.2→372.1; 404.2→344.2 / 60; 60 / 19; 27 / 0.2-15 / 0.5 / 95.7 (24.5) / 24.2
Testosterone / 7.2 / 289.0→97.0; 289.0→109.0 / 116; 116 / 29; 37 / 0.5-29 / 1 / 109.2 (16.6) / 25.3
Drospirenone / 7.2 / 367.0→91.0; 367.0→77.0 / 121; 121 / 83; 107 / 0.4-28 / 1 / 107.7 (24.4) / 19.2
Triadimenol / 7.2 / 296.0→70.0; 296.0→99.0 / 126; 126 / 41; 21 / 0.5-30 / 1 / 105.5 (17.1) / 15.1
Acetochlor / 7.4 / 270.1→224.0; 270.1→148.0 / 71; 71 / 15; 27 / 0.4-28 / 1 / 73.3 (18.2) / 23.6
Quizalofop / 7.4 / 345.2→299.2; 345.2→273.1 / 60; 60 / 23; 25 / 1-82 / 2 / 103.5 (14.4) / 6.4
Levonorgestrel / 7.4 / 313.0→91.0; 313.0→155.0 / 131; 131 / 67; 95 / 0.5-29 / 1 / 66.9 (21.6) / 22.8
Diclofenac / 7.5 / 296.0→214.0; 296.0→250.0 / 71; 71 / 49; 17 / 1-55 / 2 / 101.0 (23.7) / 15.8
Clofentezine / 7.9 / 305.0→102.0; 305.0→138.0 / 71; 71 / 57; 29 / 0.5-30 / 1 / 57.8 (24.4) / 20.9
Progesterone / 7.9 / 315.0→97.0; 315.0→107.0 / 141; 141 / 31; 37 / 0.5-30 / 1 / 101.8 (23.2) / 19.2
Phoxim / 7.9 / 298.9→96.9; 298.9→129.0 / 66; 66 / 31; 19 / 0.5-30 / 1 / 118.0 (24) / 22.5
Chlorfenvinphos / 7.9 / 361.0→99.0; 361.0→155.0 / 111; 111 / 45; 19 / 1-12 / 1 / 77.6 (11.4) / 18.1
Prochloraz / 7.9 / 378.0→310.0; 378.0→267.0 / 61; 61 / 17; 23 / 0.5-30 / 1 / 70.9 (24.5) / 20.3
Diflufenican / 8.1 / 395.1→266.1; 395.1→246.1 / 60; 60 / 39; 41 / 1-29 / 3 / 60.7 (18.0) / 19.5
Fenofibrate / 8.3 / 361.0→233.0; 361.0→139.0 / 81; 81 / 25; 45 / 1-19 / 2 / 49.0 (10.7) / 19.7
Piperonyl butoxide / 8.3 / 356.0→177.0; 356.0→119.0 / 61; 61 / 23; 49 / 0.5-3 / 1 / 82.0 (10.2) / 22.3
4-Methylbenzyliden camphre / 8.4 / 255.0→105.0; 255.0→91.0 / 41; 41 / 40; 40 / 0.5-29 / 1 / 57.1 (17.4) / 19.3
Hexythiazox / 8.4 / 353.0→228.0; 353.0→168.0 / 56; 56 / 23; 37 / 0.4-9 / 1 / 27.3 (17.5) / 21.9
Irganox 1076 / 10.0 / 549.0→149.0; 549.0→107.0 / 46; 46 / 23; 103 / 6-390 / 9 / 75.5 (20.3) / 12.9
Internal standards
Acetaminophen-d3 / 1.3 / 154.5→111.0 / 81 / 23
Enrofloxacin-d5 / 2.2 / 365.0→321.2 / 81 / 29
Carbendazim-d4 / 2.3 / 195.9→164.0; 195.9→136.2 / 96; 96 / 29; 43
Sulfamethoxazole-d4 / 2.7 / 258.0→160.1 / 81 / 23
Phenacetin-C13 / 3.4 / 181.0→110.0 / 106 / 27
3,4-Dichloroaniline-d2 / 4.5 / 165.0→131.0; 165.0→129.0 / 91; 91 / 31; 31
Carbamazepine-d10 / 5.3 / 247.2→204.2 / 116 / 29
Atrazine-d5 / 5.6 / 221.0→179.1 / 180 / 47
Diuron-d6 / 5.6 / 239.0→78.0 / 180 / 47
Androstenedione-d7 / 7.0 / 295.1→129.0 / 61 / 23
Acetochlor-d11 / 7.4 / 281.0→235.2 / 71 / 15
Diclofenac-d4 / 7.5 / 300.9→219.0 / 116 / 51
Progesterone-d9 / 7.9 / 324.1→100.1; 324.1→113.1 / 136; 136 / 31; 41
Negative ESI mode
Furosemide / 0.9 / 330.0→286.0; 330.0→205.0 / -45; -45 / -22; -22
Pravastatin / 1.6 / 423.0→321.0; 423.0→101.0 / -120; -120 / -22; -46
Pentachlorophenol / 2.4 / 265.0→35.0; 265.0→202.0 / -120; -120 / -44; -44
Ibuprofen / 2.4 / 205.2→161.0 / -40 / -18 / 0.5-10 / 1 / 102.6 (7.6) / 7.2
Bisphenol A / 2.7 / 226.9→133.0; 226.9→116.9 / -115; -115 / -34; -66 / 1-11 / 1 / 98.4 (24.5) / 14.4
17-Estradiol / 3.6 / 271.2→145.0; 271.2→183.2 / -90; -90 / -58; -56 / 0.5-30 / 1 / 93.7 (10.6) / 14.1
Estrone / 3.6 / 269.0→145.0; 269.0→143.0 / -165; -165 / -52; -76 / 2-50 / 5 / 89.0 (10.3) / 7.8
17-ethinylestradiol / 3.7 / 295.1→144.9; 295.1→143.1 / -145; -145 / -54; -76 / 0.5-10 / 1 / 86.3 (24.5) / 11.4
2,6-di-tert-butylphenol / 4.3 / 205.0→189.0 / -45 / -36 / 50-1000 / 100 / 95.1 (14.0) / 20.2
Internal standards
Phenacetin-C13 / 1.5 / 179.0→148.6 / -30 / -18
Ibuprofen-d3 / 2.4 / 208.0→164.0 / -60 / -12
Bisphenol A-d4 / 2.7 / 231.0→135.0 / -50 / -26
17-ethinylestradiol-d4 / 3.7 / 299.0→217.0 / -50 / -16
17-Estradiol-d2 / 3.6 / 273.0→147.1; 273.0→185.0 / -190; -190 / -50; -56
Table S2
Retention time (Rt) during the GC-ToF-MS, masses used for quantification and confirmation, linear range, limit of quantification (LOQ), recoveries, percentage of relative standard deviation (%RSD) and repeatability expressed as the %RSD.
Compounds / Rt(min) / Quantification mass
(Da) / Confirmation mass
(Da) / Linear range
(ng/L) / LQ
(ng/L) / Recoveries
(%RSD)
at 100xLOQ / % RSD
(at LOQ)
Biphenyl / 6.9 / 153.0704 / 154.0783 / 2.6 - 260 / 5 / 59.7 (27) / 4.0
Trifluraline / 7.7 / 306.0702 / 264.0234 / 1.6 - 160 / 3 / 80.7 (6) / 11.8
Chlorpyriphos-ethyl / 10.2 / 313.9574 / 196.9202 / 7.5 - 750 / 15 / 84.5 (13) / 11.2
Procymidon / 11.0 / 283.0167 / 96.0575 / 2.5 - 250 / 5 / 95.9 (6) / 4.9
Fluoranthene / 11.5 / 202.0783 / 200.0626 / 0.5 - 55 / 1 / 75.2 (7) / 9.1
Fenarimol / 17.0 / 219.0325 / 251.003 / 49.5 - 4950 / 100 / 109.4 (20) / 4.6
Benzo(b)fluoranthene / 19.2 / 252.0939 / 250.0783 / 2.4 - 240 / 4 / 22.6 (8) / 4.9
Benzo(a)pyrene / 20.7 / 252.0939 / 250.0783 / 3.5 - 350 / 7 / 10.1 (29) / 5.2
Internal standards
Phenanthrene-d10 / 9.4 / 188.1410 / 187.1351
Fluoranthene-d10 / 11.5 / 212.1410 / 213.1400
Table S3
Summary of the results for the selected organic micropollutants in the 80 groundwaters.
main use / frequence / max / average / median(n) / (ng/L) / (ng/L) / (ng/L)
Bisphenol A / production of plastics and resins / 77 / 7400.0 / 337.1 / 27.4
Caffeine / stimulant / 73 / 1240.0 / 106.9 / 19.8
Carbamazepine / anti-epileptic / 45 / 22.2 / 2.3 / 0.7
Pentachlorophenol / pesticide / 44 / 418.0 / 55.3 / 15.5
Ibuprofen / non-steroidal anti-inflammatory / 34 / 36.4 / 3.5 / 2
Atrazine / pesticide / 30 / 420.0 / 39.3 / 8.8
Progesterone / natural progestagen / 29 / 41.2 / 15.5 / 2
Acetaminophen / analgesic, antipyretic / 26 / 148.8 / 33.7 / 19.1
Diclofenac / non-steroidal anti-inflammatory / 17 / 120.0 / 18.8 / 5.7
4-androstenedione / natural androgen / 16 / 21.0 / 5.4 / 4
Diuron / pesticide / 13 / 258.0 / 35.2 / 18.2
Carbendazim / pesticide / 13 / 27.0 / 4.1 / 1
Azoxystrobine / pesticide / 10 / 3.3 / 1.3
Testosterone / natural androgen / 9 / 21.0 / 7.4
Ofloxacin / antibiotic / 9 / 204.0 / 64.4
Metazachlor / pesticide / 8 / 5.2 / 6.6
Drospirenone / contraceptive / 8 / 19.6 / 6.1
Bezafibrate / lipid regulator / 8 / 4.6 / 2.4
Piperonyl butoxide / pesticide synergistic / 7 / 22.0 / 7.1
Norethindrone / contraceptive / 7 / 35.0 / 14.9
Estrone / natural estrogen / 5 / 90.0 / 48.3
Sulfamethoxazole / antibiotic / 5 / 35.4 / 8.9
Levonorgestrel / contraceptive / 4 / 50.6 / 14.9
Ethinylestradiol / contraceptive / 4 / 22.0 / 12.5
Trimethoprim / antibiotic / 4 / 2.2 / 1.7
Atenolol / -blocker / 3 / 7.3 / 4.9
Norfloxacin / antibiotic / 3 / 39.0 / 39.0
Diflufenican / pesticide / 2 / 50.0
Sulfamethazine / antibiotic / 2 / 4.4 / 3.7
17-beta-Estradiol / natural estrogen / 2 / 2.3 / 1.8
Fenarimol / pesticide / 1 / 121.2
Ciprofloxacin / antibiotic / 1 / 10.0
Phoxime / pesticide / 1 / 8.0
Fluoranthene / HAP / 1 / 7.0
Metronidazole / antibiotic / 1 / 5.0
Triadimenol / pesticide / 1 / 3.7
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