聚酰亚胺固相萃取搅拌棒的制备及其在环境水中酚类的分析应用

利用相转换法制备了聚酰亚胺吸附萃取搅拌棒,用5种有机酚作为评价标样,并与现有商品化吸附萃取搅拌棒进行比较。优化了萃取搅拌速度、溶液离子强度、萃取温度、萃取时间以及热解析温度和时间。在最佳实验条件下,100 mL 样品,30% NaCl,在25℃下,经活化5 min 后的聚酰亚胺吸附搅拌棒萃取30 min (800 r/ min),然后300℃热解析4 min,使目标物脱附,再进行色谱分析。目标物在大于两个数量级浓度范围内具有良好的线性(R≥0.9995),定量限(LOQ,S/ N=10)为0.028~0.123μg/ L,重复性为1.6%~9.7%。将SBSE 与气相色谱-质谱联用,对海水、自来水和污水中的酚类进行定性与定量分析,结果表明,聚酰亚胺吸附萃取搅拌棒具有良好的选择性,最高热解析温度350℃,在分析水中痕量极性化合物领域具有广阔应用前景。

Preparation and Application of Polyimide Coated Stir Bar for Extraction of Phenols in Environmental Water Samples

A polyimide coated stir bar for sorptive extraction (SBSE) was prepared by immersion precipitation method, and evaluated by using 5 phenols and chlorinated phenols as model samples. The extraction efficiency of the prepared stir bar was the highest compared with commercial extraction phases of SBSE. Experimental parameters including stir speed, ionic strength, extraction temperature, extraction time, desorption temperature and time were optimized. Under the optimal conditions such as 100 mL of sample, 30 g of NaCl, extraction time of 30 min, stirring speed of 800 r/ min and at 25℃, the target compounds were recovered by thermal desorption at 300℃ for 4 min, more than two orders of magnitude of linearity was obtained (R≥0. 9995), LOQs (S/ N=10) were 0. 028-0. 123 μg/ L, and RSDs were in the range of 1. 6% -9. 7% . The polyimide SBSE coupled with gas chromatography-mass spectrometry was applied to the extraction/ enrichment and analysis of phenols in real samples, including tap water, sea water, and waste water. It was found that the polyimide SBSE showed high selectivity towards polar compounds and high thermostability up to 350℃.