快速制备金属基固相微萃取金涂层用于环境水样中痕量苯并[a]芘的测定

Rapid Preparation of Au Coating of Solid-phase Microextraction on Metal Fiber for Determination of Benzo[a]pyrene in Environmental Water

本文以刻蚀不锈钢丝作为固相微萃取（SPME）纤维基体,用化学沉积技术快速制备了亚微米金颗粒涂层,与高效液相色谱（HPLC）联用,用苯并[a]芘（B[a]p）评价了SPME金涂层的萃取分离性能,优化了实验条件。实验结果表明,该金涂层与基体结合牢固、稳定性好、寿命长、制备简单。所建立的金涂层SPME-HPLC法测定B[a]p线性范围为25-5 000ng/L,检出限（S/N=3）为12.50ng/L;对于4μg/L的B[a]p溶液,制备的单一金涂层SPME-HPLC分析结果的相对标准偏差（RSD）为4.86%（n=6）,重复制备的金涂层SPME-HPLC分析结果的RSD为7.81%（n=6）。实际水样中B[a]p的加标回收率在94.25%-110.9%之间,RSD为2.67%-10.24%。

A novel Au-coated fiber of SPME was rapidly prepared with chemical deposition on the etched stainless steel wire. Its SPME performance was examined with benzo[a]pyrene coupled to HPLC. It was found that the Au-coating on the etched stainless steel wire was easy to prepare, chemically and mechanically stable and durable. Single fiber repeatability and fiber-to-fiber reproducibility were less than 4.86% and 7.81% （n= 6）, respectively. Under optimized conditions, the calibration graph was linear in the range of 25-5 000 ng/L and the limit of detection was 12.50 ng/L（S/N=3）. The analytical results of water samples showed that the recoveries ranged from 94.25%to 110.9% with RSDs from 2.67% to 10.24%. The Au coating is sensitive and suitable for the preconcentration and determination of benzo[a] pyrene in real environmental water samples.