基于改性瓜环的新型固相微萃取搅拌棒的制备及其在检测环境水样中布洛芬含量方面的应用

Preparation of a novel sorption extraction stir bar based on modified cucurbiturils and its application in the detection of ibuprofen content in environmental water samples

通过凝胶-溶胶法制备了两种新型PDMS/Hydroxylated CB[n](n=5,6)固相微萃取搅拌棒,结合高效液相色谱法测定环境水中布洛芬的含量。考察了萃取时间,萃取温度,解吸时间,盐离子强度和介质p H等实验条件对萃取效率的影响。控制溶液pH=2.0,C_(NaCl)=0.15 g·m L^(-1),在25℃下搅拌萃取30 min,用甲醇超声解吸7 min萃取效果最佳。其中PDMS/Hydroxylated CB[6]涂层的效果更好,其富集倍数可达19倍。该方法在0.05~10μg·m L^(-1)的布洛芬质量浓度范围内呈现较好的线性关系,相关系数为0.9993,检出限为1.2 ng·m L^(-1),RSD为3.1%,表明该方法具有较好的重复性和可靠性。

Two novel sorption extraction stir bars(SBSE)based on modified cucurbiturils were prepared by sol-gel technique. Combinedwith high performance liquid chromatography,the content of ibuprofen in environmental water sample was detected by the twonovel sorption extraction stir bars. The experimental conditions such as extraction time,extraction temperature and time were optimized.The SBSE operation was performed at the control solution of pH=2. 0,25 ℃,30min,and the desorption was done in methanolfor 7mins with ultrasonic waves. Compared with PDMS/ HydroxylatedCB[5],the PDMS/ HydroxylatedCB[6]coating has betterextraction effect,and its enrichment factor was19. The method shows good linear relationship in the ibuprofen concentration range of0. 05 ~10μg·mL-1 . Its correlation coefficient was 0. 9993,the detection limit is 1. 2ng·mL-1 and the RSD is 3. 1%. The results indicatethat the method has good repeatability and reliability.