期刊
MICROCHIMICA ACTA
卷 186, 期 3, 页码 -出版社
SPRINGER WIEN
DOI: 10.1007/s00604-019-3289-9
关键词
Porous material; Sample preparation; Microextraction; Membrane-protected; Liquid chromatography-tandem mass spectrometry; Endocrine disrupting compounds; Hormones; Environmental water
资金
- National University of Singapore (NUS) [143-000-023-001]
- NUS Graduate School for Integrative Sciences and Engineering
A seamless two-step extraction procedure integrating ultrasound-assisted emulsification microextraction (USAEME) and vortex-assisted micro-solid-phase extraction (-SPE) was developed. A highly porous metal-organic framework of type MIL-101(Cr) is used as the sorbent, and ultra-high-performance liquid chromatography in combination with tandem mass spectrometry is used for detection. The steroid hormones estrone 17-estradiol, estriol, and 17-ethynylestradiol were extracted from water samples by using this method. These steroids are polar and do not pass through the polypropylene membrane that is conventionally used in -SPE. In the method presented here, 1-octanol is used in USAEME to extract and pre-concentrate the steroids. This facilitates the transfer to the MIL-101(Cr) phase retained by the membrane in the subsequent -SPE step. MIL-101(Cr) was characterized by various methods, and the parameters affecting the overall extraction efficiency were optimized. Under the most favorable conditions, the limits of detection are between 0.95 and 23ngL(-1). Good intra-day and inter-day precisions were obtained, with relative standard deviations of 9.9%. Enrichment factors are between 34 and 52. The method was applied to genuine environmental water samples in which estrone was detected. Relative recoveries ranged between 85.4% and 120.8%.
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