Zhang Fan, Li Zhonghai, Zhang Ying, Huang Zhiqiang, Wang Xiaosong
Se Pu. 2014 Jul;32(7):735-40. doi: 10.3724/sp.j.1123.2014.04036.
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 0.999 9. 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.
建立了一种以单壁碳纳米管(SWCNTs)为吸附剂的固相萃取分析方法,用于气相色谱 - 质谱联用(GC - MS)同时测定山茶油中的六种邻苯二甲酸酯(PAEs)。样品用正己烷稀释,然后通过玻璃SWCNTs固相萃取(SPE)柱进行净化。采用外标法定量,在选择离子监测(SIM)模式下用GC - MS测定PAEs。对影响萃取效率的重要因素,如正己烷稀释体积、吸附剂材料类型、SWCNTs用量、洗涤液体积、洗脱液类型和体积等进行了优化。最佳条件如下:正己烷稀释体积为5 mL,SWCNTs用量为0.6 g,洗涤液为20 mL正己烷,洗脱液为5 mL甲苯。六种PAEs在0.05 mg/L至1.0 mg/L范围内具有良好的线性关系,相关系数(r)均大于0.999 9。在加标山茶油(0.05 mg/kg至1.0 mg/kg)中,六种目标物的平均回收率为86.4%至111.7%,相对标准偏差(RSDs)为4.2%至10.4%。所建立的方法准确、快速,适用于山茶油中六种PAEs的测定。