title: Online solid phase extraction with liquid chromatography-tandem mass spectrometry for determination of estrogens and glucocorticoids in water.
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.
authors: 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.
authors: Shalene Xue Lin
authors: SX
authors: Goh
authors: Water Quality Office, Public Utilities Board, 82 Toh Guan Road East, Singapore 608576, Singapore.
authors: Ankur
authors: A
authors: Duarah
authors: Water Quality Office, Public Utilities Board, 82 Toh Guan Road East, Singapore 608576, Singapore.
authors: Lifeng
authors: L
authors: Zhang
authors: 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.
authors: Shane A
authors: SA
authors: Snyder
authors: 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.
authors: Hian Kee
authors: HK
authors: Lee
mesh_terms: D057205:Automation, Laboratory; D002853:Chromatography, Liquid; D004784:Environmental Monitoring / Q000379:methods*; D045166:Estradiol Congeners; D004967:Estrogens / Q000032:analysis*; D005938:Glucocorticoids / Q000032:analysis*; D057230:Limit of Detection; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D062065:Wastewater / Q000032:analysis; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis
chemical_list: D045166:Estradiol Congeners; D004967:Estrogens; D005938:Glucocorticoids; D062065:Wastewater; D014867:Water; D014874:Water Pollutants, Chemical
keywords: Estrogens; Glucocorticoids; LC–MS/MS; Online solid phase extraction; Steroid hormones; Water