土壤中五氯酚含量的放射性内标分析方法*

南京大学学报(自然科学版) ›› 2012, Vol. 48 ›› Issue (6): 768–773.

土壤中五氯酚含量的放射性内标分析方法*

周文强**，单军，郭红岩，季荣

出版日期:2015-09-11 发布日期:2015-09-11
作者简介: (南京大学环境学院污染控制与资源化国家重点实验室，南京，210023)
基金资助:
国家高技术研究发展计划(863计划)(2007AA06Z307 )

Determination of pentachlorophenol in soil with radioactive tracer
as internal standard

Zhou Wen-Qiang，Shan Jun，Guo Honk-Yan,Ji Rong

Online:2015-09-11 Published:2015-09-11
About author: (State Key Laboratory of Pollution Control and Resource Reuse,School of the Environment,Nanjing University,
Nanjing, 210023 , China)

摘要/Abstract

摘要： 五氯酚(PCP)是一种环境内分泌干扰物，曾被广泛使用并残留在上壤环境之中.上壤中存在
的五氯酚可以在酸化后采用乙酸乙醋法进行提取，使用高效液相色谱或者气相色谱进行定量分析测定，
但是由于上壤的有机质背景比较复杂，当待测物PCP浓度较低时，提取液中的杂质对待测物的测定干
扰极大，因此必须对上壤样品提取液进行净化.参考文献中相关方法之后，实验优化了PCP提取与测定
的方法和条件，使用自制的硅胶柱对样品进行净化，利用乙酸乙醋和正己烷作为洗脱剂对样品进行梯度
洗脱.和传统的内标物不同，木研究中采用¹⁴C－放射性标记的PCP作为内标以定位净化过程中PCP的
流出组份和测定样品回收率.结果表明，¹⁴C--内标法的PCP回收率达94. 3%士2.900,净化样品可用于
HPLC测定，检出PCP的最低可测浓度达到6. 7 µg/kg上壤.相比于以¹³C-PCP作为内标的气相色谱
法，¹⁴C--内标法的分析步骤简单而又快速，实现了上壤中低浓度PCP残留的快速准确测定，为研究PCP
上壤中的归趋和转化提供了新方法.

Abstract: Pentachlorophenol(PCP)is an endocrine disrupting compound，which has been widely used and caused se
were soil contamination. PCP in soil can be extracted with ethyl acetate; however, the determination of PCP by high
performance liquid chromatography or gas chromatography may be strongly disturbed by the complexity of soil ma-
trixes and impurities in the soil extract,especially when the PCP concentration in soil is low. Thus,a purification of
the extract is needed to remove the impurities. In the present study,according to references,a method for determina-
tion of PCP in soil was optimized. A self-prepared silica gel column was used for sample purification,and PCP was e
luted with a gradient mixture of ethyl acetate and hexane. Radioactive¹⁴C-labeled PCP was applied as inner standard
to localize PCP fractions during the elution and to quantify the recovery of PCP during the sample pretreatment
process. After this purification,recovery of PCP was 94. 3%士2. 9%and PCP in the extract can be easily determined
by HPLC with a lowest detected concentration of 6. 7 µg/kg dry soil.The14C-tracer combined to HPLC determina
tion was demonstrated to be a rapid and alternative method for soil PCP analysis to has chromatography, which re
qumes a tedious purification procedure and¹³C-PCP as inner standard.

周文强**，单军，郭红岩，季荣
. 土壤中五氯酚含量的放射性内标分析方法*[J]. 南京大学学报(自然科学版), 2012, 48(6): 768–773.

Zhou Wen-Qiang，Shan Jun，Guo Honk-Yan,Ji Rong. Determination of pentachlorophenol in soil with radioactive tracer
as internal standard[J]. Journal of Nanjing University(Natural Sciences), 2012, 48(6): 768–773.

参考文献

[1]McGrath R,Singleton I. Pentachlorophcnol tram formation in soil:A toxicological assessment. Soil
Biology and Biochemistry,2000，32:1311一1314.
[2]Chung N，Aust S D. Degradation of penta-chloro-phenol in soil by Phanerochaete chrysosporium. Jour
nal of Hazardous Mazterials,1995,41:177一183.
[3]Zheng W W, Wang X, Yu H，et al. Global trends and diversity in pentachlorophenol levels in the
environment and in humans:A mcta-analysis. En- vironmental Science & Technology, 2011，45: 4668一4675.
[4]Zheng W W，Yu H , Wang X , et al. Systematic re- view of pentachlorophenol occurrence in the envi- ronment and in humans in China;Not a negligible health risk due to the reemergence of schistoso- miasis. Environment international， 2012，42:105 ~16.
[5]Wang S S, Wang F, Jiang X. Advances in study on environmental behaviors of pentachlorophenol in the soil ecosystem. Acta Ecologica Sinica, 2010,30(7);1894-1902.(王诗生，王芳，蒋新.五氯酚在上壤生态系统中的环境行为研究进展.生态学报，2010,30(7) : 1894一1902）.
[6]Agency for Zoxic Substances and Disease Registry. Toxicological profile for pentachlorophenol, http//
www. atsdr. cdc. gov/toxprofilcs/tp51, pdf,2001.
[7]Yang S Z, Han X D, Chen W. Advances in the toxicity of pcntacholrophcnol on organism.Jour- nal of Environment and Health，2005，22(5):396 一398.(杨淑贞，韩晓冬，陈伟.五氯酚对生物体的毒性研究进展.环境与健康杂志，2005,22 （5）:396一398).
[8]Xu Y，Li Z L，Chen H G, et al. Genetoxicity of sodium pentachlorophenate(Na-PCP). Journal of Nanjing University(Natural Sciences)，2007，43 (4):372-376.(徐韵，李兆利，李梅等.五氯酚钠的遗传毒性效应研究.南京大学学报(自然科学),2007,43(4):372-376).
[9]Pecchi G, Reyes P, Sanhueza P, et al. Photocatalytic degradation of pentachlorophenol on TiOy sol-gel catalysts. Chcmosphcrc,2001 ,43:141一146.
[10]Han D M, Fang G Z, Yan X P. Preparation and evaluation of a molecularly imprinted sol-gel ma- terial for online solid-phase extraction coupled with high performance liquid chromatography for the determination of trace pentachlorophenol in water samples. Journal of Chromatography A，2005，1100:131一136.
[11]Shan J，Xu J，Zhou W Q, et u1. Enhancement of chlorophcnol sorption on soil by gcophagous earthworms(Metuphire guillelrni).Chemosphere, 2011,82:156一162.
[12]Becker R, Buge H，Win T.Determination of penta- chlorophenol(PCP) in waste wood-Method compari-
son by a collaborative trial. Chemosphere, 2002，47: 1001一1006.
[13]Liu Y, Wen B,Shan X Q. Determination of pentachlo- rophenol in wastewater irrigated soils and incubated
earthworms. Talanta , 2006 , 69:1254一1259.
[14]Shan J，Wang T，Li C L，et u1. Bioaccumulation and bound-residue formation of a branched 4-non- ylphenol isomer in the gcophagous earthworm Metuphire guillelrni in a rice paddy soil. Envi- ronmental Science & Technology, 2010，44:4558 一4563.
[15]Shan J,Jiang B Q,Yu B,etal.lsomci-specific degra- dation of branched and linear 4-nonylphenol isomers
in an oxic soil. Environmental Science and Technolo- gy,2011,45;8283一8289.
[16]The Ministry of Water Resources of the People’s Re public of China. SI. 391.7-2007 Sample preparation methods for organic analysis,Part 7;Silica gel clean- up. Beijing; China Water Power Press, 2008.(中华人民共和国水利部. SI. 391.7-2007有机分析样
品前处理方法第7部分:硅胶净化法.北京:中国水利水电出版社，2008).
[17]Fu M Z. Distribution characteristics of alkylphenols in coastal and estuary environment and the ecological
risk assessment. Qingdao; College of Environmental Science and Enginecring,Ocean University of China,
2007.(傅明珠.烷基酚在近海海洋及河II环境中的浓度分布与初步生态风险评估.青岛:中国海洋大学环境科学与工程学院博士学位论文，2007 ).

Metrics

Viewed

Full text

Abstract

Cited

Shared

Discussed