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作 者:吴淑燕[1] 许茜[1,2] 陈天舒[1] 王敏[1] 殷雪琰[1] 张妮萍[1] 申艳艳[1] 温作扬[2] 顾忠泽[2]
机构地区:[1]东南大学公共卫生学院,南京210009 [2]东南大学生物电子学国家重点实验室,南京210096
出 处:《分析化学》2010年第4期503-507,共5页Chinese Journal of Analytical Chemistry
基 金:国家自然科学基金(No.50533030);江苏省科技计划(No.BK2006509)资助项目
摘 要:采用静电纺丝法制备尼龙6纳米纤维膜,结合固相膜萃取-高效液相色谱法测定了矿泉水中的双酚A。对洗脱溶剂及其体积、进样速度、样品体积、样品pH值、尼龙6纳米纤维膜的用量、及其活化方式和使用次数等影响因素进行了研究。结果表明:10mL样品调至pH8.0后,以3mL/min流速通过1.5mg尼龙6纳米纤维膜,300μL甲醇即可将膜上吸附的双酚A完全洗脱,每张膜至少可重复使用6次。在此最优化条件下,方法的线性范围为0.20~20.0μg/L;检出限为0.15μg/L,膜内和膜间的相对标准偏差均小于4.5%(n=6)。本方法应用于6种不同品牌的矿泉水中双酚A的分析测定,在1.0μg/L加标水平下,测得回收率为95.0%,双酚A测得浓度低于0.30μg/L。与固相萃取方法相比,本方法高效、环保。Electrospun nylon 6 nanofibrous membrane based on solid membrane extraction-high performance liquid chromatography(SME-HPLC) for the determination of bisphenol A(BPA) in plastic bottled drinking water was performed.Important parameters that effect extraction efficiency such as eluting agent and its volume,flow rate of sample,sample volume,pH value of sample,quality of the membrane,the form of activation and the repeatedly employing of this membrane were optimized.Results indicated that 10 mL of water sample volume with pH value of 8.0 passed through nylon 6 nanofibrous membrane(1.5 mg) at flow rate of 3.0 mL/min;and only 300μL eluent(methanol) was used.Each piece of this membrane would be used at least 6 times.Under the optimized conditions,an excellent linear relationship in the range of 0.2-20μg/L with correlation coefficients of determination(r) 0.9998 was obtained,the limits of detection(LOD) about BPA was 0.15μg/L.The repeatabilities(RSD) intra-membrane and inter-membrane with nylon 6 nanofibrours membrane were all below 4.5%(n=6) .The proposed method has been applied to the analysis of plastic bottled purified water of six different brands.Satisfactory spiked recoveries of 94.95%were obtained.BPA was lower than 0.30μg/L.A comparison among the SME using nylon 6 nanofibrous membrane and other kinds of SPE sorbents used in literatures was carried out.All the results indicated that the nylon 6 nanofiboous membrane has great potential as a novel material for the enrichment and determination of BPA in water sample.
关 键 词:尼龙6纳米纤维膜 固相膜萃取 双酚A 矿泉水 高效液相色谱
分 类 号:TS275.1[轻工技术与工程—农产品加工及贮藏工程]
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