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作 者:刘海霞[1] 郑文芳[1] 刘丽[1] 李毅[1] 王雪梅[1] 杜新贞[1]
机构地区:[1]西北师范大学化学化工学院、甘肃省生物电化学与环境分析重点实验室,甘肃兰州730070
出 处:《分析科学学报》2014年第4期457-461,共5页Journal of Analytical Science
基 金:国家自然科学基金(No.21265019)
摘 要: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.
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