On-line solid-phase extraction with on-support derivatization for high-sensitivity liquid chromatography tandem mass spectrometry of estrogens in influent/effluent of wastewater treatment plants

Salvador, Arnaud; Moretton, Cédric; Piram, Anne; Faure, R.

doi:10.1016/j.chroma.2007.01.055

Cited by 132 publications

(66 citation statements)

References 20 publications

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“…For the analysis of steroidal estrogens by LC-ESI-MS/MS, pre-column derivatization by reaction with dansyl chloride at the C-3 hydroxyl groups of these compounds is by far the most popular technique, and is now widely used in both biomedical [14,[23][24][25][26][27][28][29] and environmental [30][31][32] applications. There are, however, aspects of the analysis of estrogens as dansyl derivatives that are not desirable.…”

Section: Introductionmentioning

confidence: 99%

Analysis of steroidal estrogens as pyridine-3-sulfonyl derivatives by liquid chromatography electrospray tandem mass spectrometry

Spink

2008

Analytical Biochemistry

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Sulfonyl chlorides substituted with functional groups having high proton affinity can serve as derivatization reagents to enhance the sensitivity for steroidal estrogens in liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). The most commonly used reagent for derivatization of estrogens for LC-ESI-MS/MS is dansyl chloride. In this study, we compared dansyl chloride, 1,2-dimethylimidazole-4-sulfonyl (DMIS) chloride, pyridine-3-sulfonyl (PS) chloride, and 4-(1H-pyrazol-1-yl)benzenesulfonyl (PBS) chloride for derivatization of 17β-estradiol (E2) prior to LC-ESI-MS/MS. The product ion spectra of the dansyl and DMIS derivatives were dominated by ions representing derivatization reagent moieties. In contrast, the product ion spectrum of the PS derivative of E2 and, to a lesser extent, the PBS derivative, showed analytespecific fragment ions. Derivatization with PS chloride was therefore chosen for further investigation. The product ion spectrum of the PS derivative of E2 showed intense ions at m/z 272, assigned to the radical E2 cation, and at m/z 350, attributed to the loss of SO 2 from the [M+H] + ion. Third-stage mass spectrometry of the PS derivative of E2 with isolation and collisional activation of the m/z 272 ion resulted in steroid C and D ring cleavages analogous to those observed in electron ionization mass spectrometry. The product ion spectra of the PS derivatives of estrone, 17α-ethinylestradiol, equilin, and equilenin showed similar estrogen-specific ions. Using derivatization with PS chloride, we developed an LC-ESI-MS/MS method with multiple reaction monitoring of primary and confirmatory precursor-to-product ion transitions for the determination of E2 in serum.

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Section: Introductionmentioning

confidence: 99%

Analysis of steroidal estrogens as pyridine-3-sulfonyl derivatives by liquid chromatography electrospray tandem mass spectrometry

Spink

2008

Analytical Biochemistry

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“…However, LLE requires the use of large volumes of organic solvents and additional clean-up steps and SPE methods can be tedious and time consuming. To overcome these problems, in-tube solid-phase microextraction [13], on-line SPE [14] and stir bar sorptive extraction [15,16] have been developed successfully for the determination of these substances.…”

Section: Introductionmentioning

confidence: 99%

Trace Analysis of Fifteen Androgens in Environmental Waters by LC-ESI-MS-MS Combined with Solid-Phase Disk Extraction Cleanup

Sun

Liu

Chu

et al. 2010

Chroma

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A rapid and sensitive liquid chromatography-electrospray tandem mass spectrometry method, combined with solid-phase disk extraction cleanup, was developed and applied to the analysis of fifteen androgens in waste water. Compounds included androstenedione, androstanolone, boldenone, clostebol, danazol, 6-dehydronandrolone acetate, fluoxymesterone, methyltestosterone, nandrolone, nandrolone propionate, testosterone, testosterone acetate, testosterone propionate, trenbolone and trenbolone acetate, respectively. The overall method recoveries ranged from 78.0 to 107.7% and the limits of detection for the fifteen analytes determined in influent samples were between 0.5 and 4 ng L -1. The analysis of residual androgens was carried out in waste water obtained from the Beijing area and five analytes (androstenedione, fluoxymesterone, methyltestosterone, testosterone and nandrolone) could be detected in levels

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“…The analytes were stable in the course of the analytical cycle (inter-day, 12 h). When kept in cool and dark conditions, there were no changes even for several days (Salvador et al 2007;Watabe et al 2006;Wen et al 2006).…”

Section: Methodsmentioning

confidence: 99%

Estrogenic Profile of the Svratka and Svitava Rivers in the Brno Area

Nekvapil

Borkovcová²,

Smutná

et al. 2009

Acta Vet. Brno

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Estrogens are chemical compounds considered to be endocrine disruptors. They are thought to affect the endocrine system even at low concentrations found in water (ng·l -1 ). The aim of this work was to determine estrogenic compound levels in the rivers in the Brno area. The concentration of 17β-estradiol, ethynylestradiol, estrone and diethylstilbestrol was estimated in the water samples collected in the Svratka and Svitava rivers.Estrogens were isolated from the samples using solid-phase extraction with Oasis HLB cartridges and determined by means of reversed phase HPLC with UV detection. The detection limit of the method used was 6 ng·l -1 , repeatability expressed as RSD was 11%, and recovery was 87 -103%. Estrogen values detected ranged in the interval of 6-209 ng·l -1 , depending on the sampling site. After treatment in the sewage water treatment plant, the water displayed markedly lower levels of estrogenic compounds.The results of the experiment demonstrate that HPLC-UV is a suitable method for determination of low concentrations of estrogens in water. The sewage water treatment plant reduces concentrations of estrogens but not sufficiently to prevent their estrogenic effect on fish.

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On-line solid-phase extraction with on-support derivatization for high-sensitivity liquid chromatography tandem mass spectrometry of estrogens in influent/effluent of wastewater treatment plants

Cited by 132 publications

References 20 publications

Analysis of steroidal estrogens as pyridine-3-sulfonyl derivatives by liquid chromatography electrospray tandem mass spectrometry

Analysis of steroidal estrogens as pyridine-3-sulfonyl derivatives by liquid chromatography electrospray tandem mass spectrometry

Trace Analysis of Fifteen Androgens in Environmental Waters by LC-ESI-MS-MS Combined with Solid-Phase Disk Extraction Cleanup

Estrogenic Profile of the Svratka and Svitava Rivers in the Brno Area

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