Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (01): 21-26.DOI: 10.3724/SP.J.1123.2011.09011

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Determination of 9 residual acrylic monomers in acrylic resins by gas chromatography-mass spectrometry coupled with microwave assisted extraction

LAI Ying*, LIN Rui, CAI Luxin, GE Xiuxiu, HUANG Changchun   

  1. Technology Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2011-09-07 Revised:2011-10-13 Online:2012-01-28 Published:2012-03-01

Abstract: A reliable gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 9 residual acrylic monomers (methyl acrylate, ethyl acrylate, methyl methacrylate, ethyl methacrylate, n-butyl acrylate, butyl methacrylate, styrene, acrylic acid and methacrylic acid) in acrylic resins. Solid resin was precipitated with methanol after microwave assisted extraction with ethyl acetate for 30 min, and liquid resin was diluted with methanol directly. The nine acrylic monomers got a good separation within 20 min on a DB-WAX column. The limits of quantification (LOQs, S/N=10) of the method were in the range of 1~10 mg/kg for liquid resin and 3~50 mg/kg for solid resin. The calibration curves were linear within 1~500 mg/L range with correlation coefficients above 0.995. The recoveries ranged from 84.4%to 108.6% at five spiked levels. The sensitivity, recovery and selectivity of the method can fully meet the requirements of practical work.

Key words: acrylic resin, gas chromatography-mass spectrometry (GC-MS), monomer, microwave assisted extraction