All chemicals and solvents were obtained from commercial suppliers and used without further purification, unless specified. DO2A-tert-butyl ester and 2-chlorotrityl chloride resin were purchased from Chematech (Dijon, France) and Advanced Chemtech (Louisville, KY, USA), respectively. The peptide sequence was synthesized manually using standard solid phase synthesis protocols. 1H NMR spectra were recorded at 600 MHz on Bruker AMX600 spectrometers (Delft, The Netherlands) and 13C NMR at 15 MHz on Nanalysis 60PRO (Calgary, Canada) at ambient temperature in CDCl3 unless specified. The chemical shifts (δ) for 1H and 13C are quoted relative to residual signals of the solvent on the ppm scale. Coupling constants (J values) are reported in Hertz (Hz) and are H-H coupling constants unless otherwise stated. Quality control was performed by LC-MS using an Agilent 1260 Infinity II LC/MSD XT system (Amstelveen, The Netherlands). Electrospray ionization in positive mode was used to confirm the identity of the obtained products. Purification of the synthesized ligands were performed by preparative HPLC on an Agilent 1290 Infinity II or by semi-preparative HPLC on a Waters 2695 system (Etten-Leur, The Netherlands) equipped with a diode array detector 2998. The LC-MS and the HPLC were controlled by Agilent OpenLab CDS Chemstation or Empower 3 software, respectively.
1290 infinity 2
Manufactured by Waters Corporation
The 1290 Infinity II is a high-performance liquid chromatography (HPLC) system designed for advanced analytical applications. It features a modular architecture, precise solvent delivery, and robust performance to meet the demands of modern laboratories.
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3 protocols using 1290 infinity 2
1
Synthesis and Purification of Ligands
2
Estrogenic Substance Analysis by LC-MS/MS
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In parallel to bioassays, extracts were investigated by LC‐MS/MS and analyzed for the target estrogenic substances E1, E2, EE2, E3, BPA, and 4‐tert‐octylphenol. We used a method that was previously validated by comparing estrogenicity data (n = 33 effluent and surface water samples) with that of two other laboratories (see Könemann et al., 2018 (link)). Chemical analysis was performed in negative mode with an electrospray ionization source on an Agilent G6495A triple quadrupole mass spectrometer coupled to an ultrahigh performance liquid chromatography (UHPLC) system for chromatographic separation (Agilent 1290 Infinity II, Waters Acquity UPLC BEH Shield RP18, 130 Å, 2.1 mm × 100 mm, 1.7 µm column [p/n 186002854] with a 5‐mm precolumn [p/n 186003977]). A methanol/water + 5 mM NH3 gradient was applied as described in detail in Könemann et al. (2018 (link)) and Simon et al. (2019 (link)).
3
UPLC-MS/MS Analysis of Deltamethrin
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UPLC-MS/MS analysis was carried out with slight modifications as previously described (Manjon et al., 2018) (link). Briefly, for the chromatography on an Agilent 1290 Infinity II, a Waters Acquity HSS T3 column (2.1 x 50 mm, 1.8 mm) with 2 mM ammonium-acetate in methanol and 2mM ammonium-acetate in water as the eluent in gradient mode was employed. After positive electrospray ionization, ion transitions were recorded on a Sciex API6500 Triple Quad. Deltamethrin and 4'OH deltamethrin were measured in positive ion mode (ion transitions: deltamethrin 523.000 > 281.000, 4'OH deltamethrin 539.000 > 281.000). The peak integrals were calibrated externally against a standard calibration curve.
The linear ranges for the quantification of deltamethrin and 4'OH deltamethrin were 0.5 -100 ng/mL and 0.1 -200 ng/mL, respectively. Samples were diluted prior to measurement if needed. The experiment was replicated thrice.
The linear ranges for the quantification of deltamethrin and 4'OH deltamethrin were 0.5 -100 ng/mL and 0.1 -200 ng/mL, respectively. Samples were diluted prior to measurement if needed. The experiment was replicated thrice.
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