Zhao Haixiang, Jia Yanxia, Ding Mingyu, Sun Dajiang, Zhao Mengbin
Department of Chemistry, Hebei North University, Zhangjiakou 075000, China.
Se Pu. 2011 May;29(5):443-9. doi: 10.3724/sp.j.1123.2011.00443.
A multi-residue analytical method based on solid-phase extraction (SPE) with multiwalled carbon nanotubes (MWCNTs) as adsorbent was developed. The determination of 6 organochlorine pesticides and 7 pyrethroid pesticides in vegetables (including cucumber, cherry tomato, cabbage, lettuce, purple cabbage, leek, shallot and onion) was carried out by gas chromatography-electron capture detection (GC-ECD). The GC-ECD method used two columns (HP-50 and HP-1) and two ECD detectors. The HP-50 column was used for the analysis and the HP-1 column for validation. The clean-up conditions were optimized. The analytes were extracted by acetonitrile, and the extract was cleaned up by the MWCNTs SPE cartridge. The extract was re-dissolved by hexane, eluted with acetone-hexane (7:3, v/v) from the columns. The recoveries were over 70% for the 11 pesticides in the 13 pesticides. The results indicated that the MWCNTs SPE cartridge was efficient for 8 vegetable samples, because it reduced the contamination of the coloring materials to GC-ECD. The experimental results showed the MWCNTs SPE cartridge can adsorb the coloring materials and the eluant was nearly colorless.
建立了一种以多壁碳纳米管（MWCNTs）为吸附剂的基于固相萃取（SPE）的多残留分析方法。采用气相色谱 - 电子捕获检测（GC - ECD）法测定蔬菜（包括黄瓜、樱桃番茄、卷心菜、生菜、紫甘蓝、韭菜、葱和洋葱）中的6种有机氯农药和7种拟除虫菊酯类农药。GC - ECD方法使用两根色谱柱（HP - 50和HP - 1）和两个ECD检测器。HP - 50柱用于分析，HP - 1柱用于验证。对净化条件进行了优化。分析物用乙腈提取，提取物用MWCNTs固相萃取柱净化。提取物用己烷重新溶解，用丙酮 - 己烷（7:3，v/v）从柱上洗脱。13种农药中的11种农药回收率超过70%。结果表明，MWCNTs固相萃取柱对8种蔬菜样品有效，因为它减少了色素对GC - ECD的污染。实验结果表明，MWCNTs固相萃取柱能吸附色素，洗脱液几乎无色。
