Centres for Analysis and Synthesis, Department of Chemistry, Lund University, Lund, Sweden.
Anal Chim Acta. 2012 Feb 3;713:79-85. doi: 10.1016/j.aca.2011.11.046. Epub 2011 Dec 2.
A method based on hollow fiber liquid phase microextraction (HF-LPME) for analysis of pinic acid and pinonic acid was developed and for the first time successfully applied to ambient aerosol samples. In this method, the aerosol samples were dissolved in 0.05 M H(2)SO(4) and the solution was extracted using three-phase HF-LPME where donor phase was 0.1 M (NH(4))(2)CO(3). Different parameters like type of organic solvent for membrane phase, extraction time and stirring speed etc. were optimized. Optimum extraction time was 4.5 h and optimum-stirring speed was found to be 900 rpm. We used 6-undecanone as organic phase along with tri-n-octylphosphine oxide (optimum TOPO contents was 15% w/v), which gave an enormous enrichment for both pinic and pinonic acid. Enrichment factors of 28,050 and 27,400 times were obtained for pinonic acid and pinic acid, respectively, that are the highest ever published. The extraction efficiency for pinic acid and pinonic acid were 68.5% and 70.1%, respectively. Very low limits of detection were obtained. Values of 1.0 ng L(-1) and 0.5 ng L(-1) in aqueous solutions, corresponding to 24 pg m(-3) and 12 pg m(-3) in aerosol samples were the limits of detections for pinonic acid and pinic acid, respectively. Both pinonic acid and pinic acid were found in all aerosol samples analyzed.
一种基于中空纤维液相微萃取（HF-LPME）的方法被开发出来，用于分析苍术酸和苍术酮，并首次成功应用于环境气溶胶样品。在这种方法中，气溶胶样品溶解在 0.05 M H(2)SO(4)中，然后使用三相 HF-LPME 进行萃取，其中供体相为 0.1 M (NH(4))(2)CO(3)。优化了不同的参数，如膜相的有机溶剂类型、萃取时间和搅拌速度等。最佳萃取时间为 4.5 小时，最佳搅拌速度为 900 rpm。我们使用 6-十一酮作为有机相，并加入三正辛基氧化磷（最佳 TOPO 含量为 15% w/v），这对苍术酸和苍术酮都有很大的富集作用。苍术酮和苍术酸的富集因子分别为 28050 和 27400 倍，这是迄今为止报道的最高值。苍术酸和苍术酮的萃取效率分别为 68.5%和 70.1%。检测限非常低。在水溶液中的检测限分别为 1.0 ng L(-1)和 0.5 ng L(-1)，相当于气溶胶样品中的 24 pg m(-3)和 12 pg m(-3)，这是苍术酮和苍术酸的检测限。在分析的所有气溶胶样品中都发现了苍术酸和苍术酮。
