HPLC Determination of Polycyclic Aromatic Hydrocarbons in Sediment with Ultrasonic Extraction
摘 要
提出了高效液相色谱法测定沉积物中多环芳烃(PAH′s)含量的方法。样品中多环芳烃用正己烷-丙酮(1+1)混合溶液超声提取,离心分离后,所得萃取液经蒸发浓缩,然后过装有1 g无水硫酸钠和2 g硅胶的层析柱净化。以Varian PAHs色谱柱为分离柱,不同比例配成的甲醇和水为流动相梯度洗脱,用荧光检测器检测。方法的检出限(3S/N)在0.34~1.52 ng·g-1之间。方法用于沉积物中多环芳烃的测定,测定结果的相对标准偏差(n=5)在3.2%~10.6%之间。用标准加入法测定方法的回收率,结果在57.1%~103.4%之间
Abstract
Contents of polycyclic aromatic hydrocarbons (PAH′s) in sediment were determined by HPLC. The PAH′s in the sample were extracted ultrasonically with a mixture of n-hexane-acetone (1+1). After centrifugation, the extract was evaporated, concentrated and purified with chromatographic column packed with 1 g of Na2SO4 and 2 g of silica gel. Varian PAHs chromatographic column was used as stationary phase, and solutions of methanol mixed with water in different ratios were used as mobile phase in the gradient elution. The eluate from the column was used for HPLC analysis with fluorescence detector. Detection limits (3S/N) of the method found were in the range of 0.34-1.52 ng·g-1. The proposed method was used in determination of PAH′s in sediment, giving values of RSD′s (n=5) in the range of 3.2%-10.6%. Recovery found by standard addition method were in the range of 57.1%-103.4%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 河南省重点科技攻关项目(No.072102350025);河南省教育厅自然科学基础研究计划(2009A610007)
收稿日期 2011/2/16
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备注冯精兰(1979-),女,河南新乡人,副教授,主要研究方向为环境化学。
引用该论文: FENG Jing-lan,ZHAI Meng-xiao,SHEN Jun-hui,SUN Jian-hui. HPLC Determination of Polycyclic Aromatic Hydrocarbons in Sediment with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(3): 308~311
冯精兰,翟梦晓,申君慧,孙剑辉. 超声萃取-高效液相色谱法测定沉积物中多环芳烃[J]. 理化检验-化学分册, 2012, 48(3): 308~311
被引情况:
【1】张辰凌,桂建业,张莉,张永涛,李晓亚,赵国兴,田来生, "超声衍生萃取-气相色谱-质谱法测定土壤中茅草枯含量",理化检验-化学分册 50, 452-454(2014)
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参考文献
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【2】KIM G B, MARUYA K A, LEE K A, et al. Distribution and sources of polycyclic aromatic hydrocarbons in sediments from Kyeonggi Bay, Korea[J]. Mar Pollut Bull, 1999,38:7-15.
【3】KUBICKI J D. Molecular simulations of Benzene and PAH interactions with soot[J]. Environ Sci Techno, 2006,40:2298-2303.
【4】DOICK K J, BURAUEL P, JONES K C, et al. Distribution of aged 14C-PCB and 14C-PAH residues in particle-size and humic fractions of an agricultural soil[J]. Environ Sci Techno, 2005,39:6575-6583.
【5】RICHTER P, JIMENEZ M, SALAZAR R, et al. Ultrasound assisted pressurized solvent extraction for aliphatic and polycyclic aromatic hydrocarbons from soils[J]. J Chromatogr A, 2006,1132:15-20.
【6】胡国成,郭建阳,罗孝俊,等.白洋淀表层沉积物中多环芳烃的含量、分布、来源及生态风险评价[J].环境科学研究, 2009,22(3):321-326.
【7】宋冠群,林金明.环境样品中多环芳烃的前处理技术[J].环境科学学报, 2005,25(10):15-20.
【8】刘爱霞,郎印海,薛荔栋,等.日照近岸海域表层沉积物中多环芳烃的生态风险分析[J].环境化学,2008,27(6):805-809..
【9】BOSSIO J P, HARRY J, KINNEY C A. Application of ultrasonic assisted extraction of chemically diverse organic compounds from soils and sediments[J]. Chemosphere, 2008,70:858-864.
【10】蒋敏谢,孟峡,谢芳.沉积物中有机成分的分析方法研究[J].北京师范大学学报, 2002,38(3):370-376.
【11】漆新华,庄源益.超临界流体技术在环境科学中的应用[M].北京:科学出版社, 2005.
【12】董新艳,杨亦文,任其龙.复杂基体中痕量多环芳烃分析测定方法的研究进展[J].色谱, 2005,11(6):609-615.
【13】韩豫萍,项伟,孙汉董.多环芳烃类有机污染物的采样和预处理技术[J].云南化工, 2002,10(5):37-39.
【14】饶竹,李松,何淼,等.高效液相色谱-荧光-紫外串联测定土壤中16种多环芳烃[J].分析化学, 2007,7(7):954-958.
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