Determination of Steroidal Estrogens in Flushed Dairy Manure Wastewater by Gas Chromatography‐Mass Spectrometry

Abstract

There is a critical need to accurately measure the concentrations of natural steroidal estrogens in flushed dairy manure wastewater (FDMW) to assess any potential risk of waterway contamination resulting from land application. Estrogens are a concern because low concentrations (10-100 ng L-1) in water can adversely affect aquatic vertebrate species such as fish, turtles, and frogs by disrupting the normal function of their endocrine systems. The objective of this study was to develop a sample preparation method that permits the quantification of four natural steroidal estrogens (17alpha-estradiol, 17beta-estradiol, estrone, and estriol) in FDMW by gas chromatography-mass spectrometry (GC-MS). Solid-phase extraction with graphitized carbon black was used for the bulk extraction of estrogens from FDMW and additional sample purification was accomplished with C-18. The sample preparation method allowed estrogens to be detected accurately by GC-MS in FDMW. Spiked recovery experiments indicated that the method is satisfactory for measuring the estrogens of interest in FDMW with average recovery of >90%. As expected in FDMW, characterization of the estrogen profile revealed a large abundance of 17alpha-estradiol relative to 17beta-estradiol and estrone. Estriol was not detected in FDMW. The methodology developed in this research helps provide an analytical foundation for the quantification of steroidal estrogens in FDMW by GC-MS.

Determination of fecal contamination indicator sterols in an Australian water supply system

“…Sterol standards, 3β-hydroxy-5α-cholestane (cholestanol), and 5β-cholestan-3β-ol (coprostanol) were purchased from Sigma-Aldrich (Australia). Pyrelene d-12 was used as an internal standard (Hanselman et al 2006) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) derivatization reagents were also obtained from Sigma-Aldrich (Australia).…”

A yeast estrogen screen without extraction provides fast, reliable measures of estrogenic activity

“…Matrix effects are a concern with YESne because the yeast is exposed to matrix effects more with this method than in methods that extract estrogenic components from the wastewater, thus removing some of the matrix effect chemicals. However, extraction does not remove all matrix effects, and they cause interference with all methods, especially with liquid chromatography-tandem mass spectrometry (LC-MS) [34,35], gas chromatographymass spectrometry (GC-MS) [20,36], and methods using the human mammalian cell lines [37].…”

Detection of estrogenic hormone 17β-estradiol in soil samples by a recombinant yeast bioassay and supercritical fluid extraction

“…25) Sample-4 was also collected from the agricultural land around the animal house of Chonnam National University where soils are likely to receive animal manure which is a possible source of organic toxic chemicals. 26) In case of supercritical fluid extraction (SFE) method, samples SFE-4 and SFE-5 showed some activities compare to the standard after 48 h incubation (EC50 =0.205 for standard and 0.298 for SFE-4 and 0.2730 for SFE-5) but the color development in the microtitre plate was not that intense compare to the color developed by M-3 and M-4. After 72 h incubation, the soil sample SFE-1 produced similar color development to that of M-4 and M-3 in the microtitre plate ( Fig.…”