期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1233, 期 -, 页码 1-7出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2012.01.064
关键词
Hollow fiber solvent-stir bars microextraction (HF-SSBME); Anabolic steroids; Gas chromatography-mass spectrometry; Sample preparation
资金
- Ministry of Education of China [708056]
- Education Bureau of Fujian Province [HX2005-74]
In this paper, a convenient and self-assembled hollow fiber solvent-stir bar microextraction (HF-SSBME) device was developed, which could stir by itself. In the extraction process, the proposed device made the solvent bar not floating at the sample solution and exposing to air while organic solvents outside hollow fiber always wrapped with donor phase solvent, which reduced the vaporization of organic solvents. This design could improve the precisions and recoveries of experiments. For evaluating the device, seven anabolic steroids (prasterone, 5 alpha-androstane-3 alpha, 17 beta-diol, methandriol, 19-norandrostenediol, androstenediol, methyltestosterone and methandienone) were used as model analytes and extraction conditions such as type and volume of organic solvents, agitation speed, extraction time, extraction temperature and salt addition were studied in detail. Under the optimum conditions (15 mu L toluene, 40 degrees C, stirring at 750 rpm for 30 min with 1.5g sodium chloride addition in 20.0 mL donor phase), the linear ranges of anabolic steroids were 0.25-200 ng mL(-1) with gas chromatography-mass spectrometry. The limits of detection were lower than 0.10 ng mL(-1). The recoveries and precisions in spiked urine and hair samples were between 73.97-93.56% and 2.18-4.47% (n = 5). HF-SSBME method combined the intrinsical merits of hollow fiber with the superiority of the proposed self-stirring device which can be developed to two-phase, three-phase and in situ derivatization modes with wide prospect of application. Besides, the pedestal of this proposed device can be converted to fix stir bar in stir bar sorptive extraction (SBSE) method. (C) 2012 Elsevier B.V. All rights reserved.
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