Citation: ZHANG Fan, LI Zhonghai, ZHANG Ying, HUANG Zhiqiang, WANG Xiaosong. 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[J]. Chinese Journal of Chromatography, ;2014, 32(7): 735-740. doi: 10.3724/SP.J.1123.2014.04036 shu

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

1.
1. Faculty of Food Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China;

Corresponding author: HUANG Zhiqiang,
Received Date: 23 April 2014
Available Online: 19 May 2014
Fund Project: 国家科技支撑计划课题(2012BAK08B01) (2012BAK08B01)国家质检总局科技计划项目(2013IK160) (2013IK160)湖南省研究生科研创新基金项目(CX2012B332). (CX2012B332)

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