Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, PR China; University of Chinese Academy of Sciences, Beijing 100039, PR China.
Talanta. 2013 Nov 15;116:188-94. doi: 10.1016/j.talanta.2013.05.025. Epub 2013 May 16.
A mixed matrix membrane (MMM), based on carbon nanotubes (CNTs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine strychnine and brucine in urine. This MMM was prepared by dispersing CNTs in water via surfactant assistance, and then immobilizing CNTs into the pores of HF by capillary forces and sonification. The prepared carbon nanotubes reinforced hollow fiber (CNTs-HF) was subsequently wetted by a few microliters of organic solvent (1-octanol), and then applied to extract the target analytes in direct immersion sampling mode. After extraction, analytes were desorbed via ultrasonic-assisted effect, and then detected via high-performance liquid chromatography (HPLC). To achieve the highest extraction efficiency, main extraction parameters such as the type and amount of surfactant, the diameter and doping level of CNTs, extraction time, desorption condition, pH value, stirring rate and volume of the donor phase were optimized. Under the optimum extraction conditions, the method showed good linearity ranges with correlation coefficients higher than 0.9990, good repeatability and batch-to-batch reproducibility with relative standard deviations (RSDs) less than 6% and 5% for strychnine and brucine, respectively, and low limits of detection (0.7 and 0.9 µg L(-1) for strychnine and brucine, respectively). The recoveries were in the range of 83.81-116.14% at three spiked levels. The developed method was successfully applied to real urine sample with mean relative recoveries of 94.28% and 91.30% for strychnine and brucine, respectively. The developed method shows comparable results against reference methods and is a simple, green, and cost-effective microextraction technique.
一种基于碳纳米管(CNTs)和中空纤维(HF)的混合基质膜(MMM)被制备出来,并与固相微萃取(SPME)模式相结合,用于测定尿液中的士的宁和马钱子碱。这种 MMM 是通过在表面活性剂的帮助下将 CNTs 分散在水中,然后通过毛细作用力和超声将 CNTs 固定在 HF 的孔中而制备的。制备的碳纳米管增强型中空纤维(CNTs-HF)随后被几微升有机溶剂(1-辛醇)润湿,然后应用于直接浸入式采样模式下提取目标分析物。萃取后,通过超声辅助作用解吸分析物,然后通过高效液相色谱(HPLC)检测。为了获得最高的萃取效率,优化了主要萃取参数,如表面活性剂的类型和用量、CNTs 的直径和掺杂水平、萃取时间、解吸条件、pH 值、搅拌速度和供体相的体积。在最佳萃取条件下,该方法具有良好的线性范围,相关系数均高于 0.9990,具有良好的重复性和批间重现性,士的宁和马钱子碱的相对标准偏差(RSD)分别小于 6%和 5%,检测限低(士的宁和马钱子碱分别为 0.7 和 0.9 µg L(-1))。在三个加标水平下,回收率在 83.81-116.14%之间。该方法成功应用于真实尿样,士的宁和马钱子碱的平均相对回收率分别为 94.28%和 91.30%。与参考方法相比,该方法具有相当的结果,是一种简单、绿色、经济有效的微萃取技术。