Preparation of solid-phase microextraction fibers by in-mold coating strategy for derivatization analysis of 24-epibrassinolide in pollen samples

J Chromatogr A. 2012 Nov 2:1262:49-55. doi: 10.1016/j.chroma.2012.09.008. Epub 2012 Sep 10.

Abstract

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 μg/L with the detection limit of 0.13 μg/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.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Biotechnology / instrumentation
  • Biotechnology / methods
  • Brassica rapa / chemistry
  • Brassinosteroids / analysis*
  • Brassinosteroids / isolation & purification
  • Chromatography, High Pressure Liquid
  • Helianthus / chemistry
  • Limit of Detection
  • Pollen / chemistry*
  • Polyethylene Glycols / chemistry
  • Polymethacrylic Acids / chemistry
  • Reproducibility of Results
  • Solid Phase Microextraction / instrumentation*
  • Solid Phase Microextraction / methods
  • Steroids, Heterocyclic / analysis*
  • Steroids, Heterocyclic / isolation & purification

Substances

  • Brassinosteroids
  • Polymethacrylic Acids
  • Steroids, Heterocyclic
  • Polyethylene Glycols
  • brassinolide