摘要
建立了高效液相色谱-荧光检测法同时测定环境水体中双酚A(BPA)、辛基酚(DP)和壬基酚(NP)的方法。比较了液液萃取(LLE)和固相萃取(SPE)两种前处理方法,并设计了供复杂样品使用的净化柱。水样经萃取后,用轻柔氮气吹干,甲醇溶解,采用Phenomenex Luna C18色谱柱,以乙腈-水为流动相进行梯度洗脱,在激发波长275nm、发射波长300nm下进行荧光检测。结果表明,BPA、NP、OP的仪器检出限(S/N=3)分别为1μg/L、2μg/L和1μg/L。SPE法操作简单快捷,虽然NP、OP的回收率低于LLE法,但仍能满足对环境样品的测定要求。净化柱净化效果较好,能够进一步去除基质干扰,满足特别复杂水样的前处理。方法基于不同样品处理的浓缩倍数不同,三种物质的检出限在0.001~0.004μg/L之间。环境水样中BPA、NP和OP的加标回收率分别为86.2%~104%、61.6%~109%和81.5%~100%,相对标准偏差(RSD)分别为2.9%~6.4%、2.4%~5.6%和2.7%~6.9%。
Methods for the simultaneous determination of bisphenol A (BPA), octylphenol (OP) and nonylphenol (NP) in environmental water have been developed by high performance liquid chromatography(HPLC) with a fluorescence detector. Effect of two pretreatment methods including liquid-liquid extraction technique with dichloromethane and solid phase extraction technique with C18 were compared and a specially designed glass cleanup column would be used for samples with complex matrix. The extracts of the water samples were evaporated with a stream of nitrogen and the residues were dissolved in methanol. For the HPLC determination, a Phenomenex Luna C18 column(150 × 2.0 mm i. d. , 5 μm) was employed and the mixture of acetonitrile-water was used as the mobile phase with a flow rate of 0.4 mL/min under fluorescence detection with excitation and emission wavelengths of 275 nm and 300 nm,respectively. The results showed that the instrument detection limits(S/N=3) of BPA, NP and OP were 1 μg/L, 2 μg/L, 1 μg/L, respectively. Although the recoveries of the targets obtained by SPE were lower than those by LLE,the former had the advantages of simple and fast operation and still met the requirements of the determination. The clean column showed a better purification effect on further removing the interference of impurities to meet sample processing. Due to the different enrichment factors of two sample pretreatment methods, the method detection limits of three targets were in the range of 0. 001-0.004 μg/L. Recoveries of sea water samples were 86.2%-104% for BPA,61.6%-109% for NP,and 81.5%-100% for OP,with the RSDs of 2.9%-6.4% ,2.4%-5.6% and 2.7%-6.9% ,respectively.
出处
《分析科学学报》
CAS
CSCD
北大核心
2013年第2期149-153,共5页
Journal of Analytical Science
基金
海洋公益性行业科研专项经费(No.201105022)
国际极地年中国行动计划项目支持
国家海洋局第三海洋研究所基本科研业务资助项目(海三科2009025)
关键词
环境激素
双酚A
辛基酚
壬基酚
高效液相色谱法
Environmental estrogens
Bisphenol A
Octylphenol
Nonylphenol
High performance liquidchromatography