期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1262, 期 -, 页码 49-55出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2012.09.008
关键词
Solid-phase microextraction; In-mold coating; Derivatization; Large volume injection; 24-Epibrassinolide
资金
- National Natural Science Foundation of China [90817012, 21127008, 21075140]
- Guangdong Provincial Natural Science Foundation of China [9251027501000004]
A novel and simple in-mold coating strategy was proposed for the preparation of uniform solid-phase microextraction (SPME) coatings. Such a strategy is based on the direct synthesis of the polymer coating on the surface of a solid fiber using a glass capillary as the mold. The capillary was removed and the polymer with well-controlled thickness could be coated on the silica fiber reproductively. Following the strategy, a new poly(acrylamide-co-ethylene glycol dimethacrylate)(poly(AM-co-EGDMA)) coating was prepared for the preconcentration of 24-epibrassinolide (24-epiBL) from plant matrix. The coating had the enrichment factor of 32 folds, and the extraction efficiency per unit thickness was 5 times higher than that of the commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating. A novel method based on SPME coupled with derivatization and large volume injection-high performance liquid chromatography (LVI-HPLC) was developed for the analysis of 24-epiBL. The linear range was 0.500-20.0 mu g/L with the detection limit of 0.13 mu g/L. The amounts of endogenous 24-epiBL in rape and sunflower breaking-wall pollens samples were determined with satisfactory recovery (77.8-104%) and reproducibility (3.9-7.9%). The SPME-DE/LVI-HPLC method is rapid, reliable, convenient and applicable for complicated plant samples. (C) 2012 Elsevier B.V. All rights reserved.
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