Chinese Journal of Chromatography ›› 2014, Vol. 32 ›› Issue (7): 735-740.DOI: 10.3724/SP.J.1123.2014.04036

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Determination of six phthalate acid esters in camellia oil by gas chromatography-mass spectrometry coupled with solid-phase extraction using single-walled carbon nanotubes as adsorbent

ZHANG Fan1,3, LI Zhonghai1, ZHANG Ying2, HUANG Zhiqiang2, WANG Xiaosong4   

  1. 1. Faculty of Food Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China;
    2. Hunan Academy of Inspection and Quarantine, Changsha 410004, China;
    3. Changsha Environmental Protection College, Changsha 410004, China;
    4. Shimadzu Enterprise Management (China) Co., Ltd., Guangzhou 510010, China
  • Received:2014-04-23 Revised:2014-05-19 Online:2014-07-08 Published:2014-06-25

Abstract:

An analytical method based on solid-phase extraction with single-walled carbon nanotubes (SWCNTs) as adsorbent was developed for the simultaneous determination of six phthalate acid esters (PAEs) in camellia oil by gas chromatography-mass spectrometry (GC-MS). The samples were diluted by hexane and then cleaned up with a glass SWCNTs solid phase extraction (SPE) column. The PAEs were measured by GC-MS in selected ion monitoring (SIM) mode, using external standard method for quantitative analysis. The important factors affecting extraction efficiency, such as the dilution volume of hexane, the type of adsorbent material, the dosage of SWCNTs, the volume of wash solution, the type and volume of elution solution were optimized. The optimal conditions were as follows: the dilution volume of hexane was 5 mL, the dosage of SWCNTs was 0.6 g, the wash solution was 20 mL hexane, and the elution solution was 5 mL toluene. The six PAEs had a good linear range from 0.05 mg/L to 1.0 mg/L, with the correlation coefficients (r) all above 0.9999. The average recoveries of the six targets in spiked camellia oil (from 0.05 mg/kg to 1.0 mg/kg) ranged from 86.4% to 111.7% with the relative standard deviations (RSDs) from 4.2% to 10.4%. The developed method is accurate, quick and suitable for the determination of the six PAEs in camellia oil.

Key words: camellia oil, gas chromatography-mass spectrometry (GC-MS), phthalate acid esters, single-walled carbon nanotubes (SWCNTs), solid-phase extraction (SPE)

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