HPLC Determination of Benzo[a]pyrene in Water with Rapid Anodization of Stainless Steel Wire as Solid-Phase Microextraction Fiber
摘 要
采用快速阳极氧化不锈钢丝作为固相微萃取纤维-高效液相色谱法测定水中苯并[a]芘的含量.结果表明:阳极氧化不锈钢丝制作简单、稳定性好、寿命长.水样用固相微萃取头在30 ℃和1 000 r·min-1搅拌速率下萃取40 min,萃取头解吸3 min.以C18反相色谱柱为分离柱,以甲醇-水(95+5)混合液为流动相进行色谱分离.在检测波长254 nm处进行测定.苯并[a]芘的质量浓度在0.1~100 μg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为10.92 ng·L-1.在10,50 μg·L-1等2个浓度水平进行加标回收试验,回收率在97.9%~110%之间.
Abstract
Stainless steel wire was rapidly anodized and use as extraction fiber in SPME separation which was combined with the HPLC determination of benzo[a]pyrene in water.It was found that the anodized stainless steel wire was easy to prepare,chemically and mechanically stable and durable.The water sample was extracted with the SPME fibrous head for 40 min at 30 ℃ with stirring at the rate of 1 000 r·min-1.The microextraction head was desorbed for 3 min.C18 reverse phase chromatographic column was used as stationary phase,and methanol-H2O (95+5) mixture was used as mobile phase in the chromatographic separation.UV-detection at 254 nm was adopted in the determination.Linear relationship between values of peak area and mass concentration of benzo[a]pyrene was kept in the range of 0.1-100 μg·L-1,with detection limit (3S/N) of 10.92 ng·L-1.Tests for recovery were made by standard addition method at the concentration levels of 10 μg·L-1 and 50 μg·L-1,giving values of recovery in the ranges of 97.9%-110%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201508033
所属栏目 专题报道(环境监测)
基金项目 国家自然科学基金项目(21265019)资助
收稿日期 2014/8/5
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联系人作者刘丽(duxz@nwnu.edu.cn)
备注刘丽(1987-),女,甘肃庆阳人,讲师,硕士,研究方向为样品前处理技术及其分析应用.
引用该论文: LIU Li,LIU Hai-xia,LI Yi,YANG Yao-xia,DU Xin-zhen. HPLC Determination of Benzo[a]pyrene in Water with Rapid Anodization of Stainless Steel Wire as Solid-Phase Microextraction Fiber[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(8): 1163~1167
刘丽,刘海霞,李毅,杨尧霞,杜新贞. 快速阳极化不锈钢丝固相微萃取-高效液相色谱法测定水中苯并[a]芘含量[J]. 理化检验-化学分册, 2015, 51(8): 1163~1167
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【7】LI Xiang,ZHONG Ming,CHEN Jian-min.Electrodeposited polyaniline as a fiber coating for solid-phase microextraction of organochlorine pesticides from water[J].J Sep Sci,2008,31(15):2839-2845.
【8】WANG Yong-hua,LI Yong-qiang,ZHANG Juan,et al.A novel fluorinated polyaniline-based solid-phase microextraction coupled with gas chromatography for quantitative determination of polychlorinated biphenyls in water samples[J].Anal Chim Acta,2009,646(1/2):78-84.
【9】CUI Xiao-yan,GU Zhi-yuan,JIANG Dong-qing,et al.In situ hydrothermal growth of metal-organic framework 199 films on stainless steel fibers for solid-phase microextraction of gaseous benzene homologues[J].Anal Chem,2009,81(23):9771-9777.
【10】ZENG Jing-bin,CHEN Jin-mei,SONG Xin-hong,et al.An electrochemically enhanced solid-phase microextraction approach based on a multi-walled carbon nanotubes/Nafion composite coating[J].J Chromatogr A,2010,1217(11):1735-1741.
【11】XU Hua-ling,LI Yan,JIANG Dong-qing,et al.Hydrofluoric acid etched stainless steel wire for solid-phase microextraction[J].Anal Chem,2009,81(12):4971-4977.
【12】CHONG S L,WANG Dong-xin,HAYES J D,et al.Sol-gel coating technology for the preparation of solid-phase microextraction fibers of enhanced thermal stability[J].Anal Chem,1997,69(19):3889-3898.
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【15】吕天峰,张宝,滕恩江,等.固相微萃取-气相色谱-质谱法测定水体中半挥发性有机污染物[J].理化检验-化学分册,2013,49(8):957-964.
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