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J Chromatogr A. 2016 Sep 23;1465:9-19. doi: 10.1016/j.chroma.2016.08.040. Epub 2016 Aug 18.

Online solid phase extraction with liquid chromatography-tandem mass spectrometry for determination of estrogens and glucocorticoids in water.

Author information

1
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore, Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
2
Water Quality Office, Public Utilities Board, 82 Toh Guan Road East, Singapore 608576, Singapore.
3
National University of Singapore, Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore; Department of Chemical & Environmental Engineering, University of Arizona, 1133 E James E Rogers Way, Harshbarger 108, Tucson, AZ, 85721-0011, USA.
4
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore, Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore. Electronic address: chmleehk@nus.edu.sg.

Abstract

The present work describes the development of a novel fully automated online solid phase extraction (SPE) coupled with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) using negative electrospray ionisation (ESI) for the simultaneous determination of six estrogens and six glucocorticoids in water. Filtered water samples (5mL) were preconcentrated on a HyperSep™ Retain PEP SPE cartridge, eluted in back-flush mode, and separated on an LC column before analysis by tandem mass spectrometry. The total analysis time for each sample was 17min. Different experimental parameters such as the type of online SPE cartridge, loading flow rate, and composition of methanol in the loading phase were optimised. The intra-day repeatability of method ranged from 1.48 to 9.68% for all analytes, and the inter-day reproducibility ranged from 2.03 to 8.63% for all analytes, except for dexamethasone at 11.95%. These were calculated based on the peak area responses of the targeted analytes spiked at 50ng/L in ultrapure water. The method also showed good linearity from 1 to 100ng/L, with the limits of detection (LODs) ranging from 0.16 to 2.14ng/L. The proposed method was applied to the analysis of municipal wastewater. This fully automated online SPE extraction coupled with LC-MS/MS method is effective and reliable to measure estrogens and glucocorticoids simultaneously due to its high throughput, relatively low solvent consumption, reusability of the online SPE cartridge, and reduction of manual labor.

KEYWORDS:

Estrogens; Glucocorticoids; LC–MS/MS; Online solid phase extraction; Steroid hormones; Water

PMID:
27562415
DOI:
10.1016/j.chroma.2016.08.040
[Indexed for MEDLINE]

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