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Evaluation of Analytical Chemical Methods for Detection of Estrogens in the Environment

Analytes Matrix Sample size Sample preparation Preconcentration (x times) LC-column Detection method LOD (ng/L) a) LOQ (ng/L)a) RSD (%) (at which concentration.) a) Recovery (%)a) Levels (ng/L) ref STP-in   0.15 L 750x 0.2- 0.6 2.4-5.6 STP-out 0.4 L 2000x 0.08- 0.2   2.7-6.2 E1, E2, EE2, E3 Surface water 4 L SPE cartridge with 0.5 g graphitized carbon black 20000x Alltima 25x4.6 RP-C18 µm ESI(-)-MS- MS (API PE Sciex 2000) 0.008- 0.02   3.1-4.8 (25) Urine 0.005 L 25x 16-70 Wastewater 0.05 L 250x 2-7 STP-in 0.100 L 500x 1-2 E1, E2, E3 + G-&S- conjugates STP-out 0.250 L SPE cartridge with 0.5 g graphitized carbon black 2500x Alltima 25x4.6 RP-C18 µm ESI(-)-MS- MS (API PE Sciex 2000) 0.3-1 3-7 76-98 n.d.-72 (69) E1, E2, E3, MeEE2, EE2, DES, progestogens STP-out and surfacte water 0.5 L C18 SPE 1000x Lichrospher 100 RP- 18/Lichrospher 60 RP-select B DAD-ESI(-)- MS 50- 500 <18% >83% n.d.-263 (24;75) STP-in   0.1 L 500x 0.4- 0.85 73-100 STP-out 0.25 L 1250x 0.04- 0.24 82-98 E1, E2, E3, EE2 + G-&S- conjugates Surface water 2 L SPE cartridge with 0.5 g graphitized carbon black 10,000x Alltima 25x4.6 RP-C18 µm ESI(-)-MS- MS (API PE Sciex 2000) 0.005- 0.03 78-100 <100 (49) E1, E2, EE2, E3, DES, progestagens Surface water 0.2 L PLRP-S cartridge b) Lichrospher 100 RP- 18/Lichrospher 60 RP-select B DAD 15 3 103-112 (101) E!, E2, EE2, E3, E2-17α, G-&S- conjugates STP-out Surface water 0.5 L EDS-1 SPE cartridge + fluorisil cartridge 1000-10,000x Waters Xterra MS C18/Zorbax, extend C18 ESI(-)-MS- MS 0.1- 1.5 3-17 77-106 0.3-34 (62) E1, E2, E2- 17α EE2, E3, progestagens Surface water, Groundwater 1 L SPE cartridge with 0.5 g graphitized carbon black 5000x Alltech, C18, 5 µm APCI(+)-MS- MS (Sciex API 365) 0.5-1 3.8-7.0 82-91 (63) E1, E2, EE2, E3 STP-in STP-out 1 L ENVI-CARB cartridge 4000x Alltima C18 column APCI(+)-MS- MS (Sciex API 365) 0.5 (E2, EE2) 1 (E1, E3) 8-11 (57) E1, E2 STP-out 1L Lichrolut+C18 SPE cartridge +Immunosorbent cartridge 5000x Betasil, C18, 3 µm, 15 cm ESI(-)-MS 0.07-0.18 <5% 92-107 (102)
E2, EE2 and phenolic EDCs STP-out, surface water 5 L Empore® disk 5000x Preparative normal phase chromatrography, polar fraction separated on phenomenex ODS C18 columns Fluorescence 229 nm excitation, 310nm emission 3.2 c) 0.8 c) 72-78 (65) E2, EE2, E3 STP-in   0.5 L 2,500x 0.4- 0.5 STP-out 1 L SPE cartridge with 0.5 g graphitized carbon black 5,000x ESI(-)-MS- MS (API PE Sciex 2000) 0.2- 0.25 <10% 88-97 (14) E1, E2, EE2, E3 Surface water   0.05 L SPE C18 cartridge 1000x Poruspher ® C18 column ESI(-)–MS ion trap 4.2- 10.6 13.9-35 <16.1% 95.8-109.5 (74) E1, E2, E2- 17α EE2, E3, MeEE2 Suface water 3.5 mL 85 µm polyacrylate SPME fibers d) Lichrospher C18 column UV-ED 70-80 <11% (intra-day) <15% (between days) (68) E2, E3, EE2 and various EDCs Surface water 0.03 L   PRP-1 SPE cartridge Nd SGE-ODS column Fluorescense 230 nm excitation, 290 nm emission 20-50 nd 100 (66) E1, E2, EE2, E3 River water STP-out water 1 L ENVI-18 cartridge (supelco) 1000x Phenomenex Luna C-18 Column ESI(-)-MS- MS (Micromass) 5   nd (103) E1, E2, EE2, E3, DES and other steroids River sediment 5 g Lyophilisation – ultrasonification extraction – C18SPE 55 e) Lichrospher C18 column DAD-ESI(-)- MS 0.05-1 ng/g 11-19 93-100 Nd<22.8 ng/L (95) E1, E2, EE2, E3, DES, other steroids, and EDC’s River sediment 5 g Lyophilisation – pressurised liquid extraction 40 e) LiChrospher ADS Lichrospher C18   RAM-LC-MS 1-5 ng/g   2.5-7.1 94-104 (96) E2, EE2 Fish estrogenicity assay 0.05-1 L Waters Sep-Pak C18 1000 mg cartridges 167-3333 Phenomenex prodigy C18 LC-APCI(+)- MS 0.6-1 13.3-13.8 78-83 (E2) 80-85 (EE2) 10-500 ng/L (104) a) Data only presented for the non-conjugated estrogens. LOQand LOD are reported for extracted and preconcentrated samples b) Samples were eluted directly into the HPLC-column c) Snyder et al. only presented LOD and LOQ for the instrument and not for the whole method. They claim that samples were preconcentrated 5000 times, however this is questionable. d) As SPME was used, the number of times the sample was preconcentrated can not be reported. e) As solid samples were analysed, the number refers to the preconcentration of the sediment-extract Abreviations: DES=diethylstilbestrol; EDCs=endocrine disrupting chemicals; ESI=electrospray ionisation; UV=ultraviolet detection; UV-ED=ultraviolet –electrochemical detection,  dw=dry weight

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