气相色谱法测定水产品中五氯酚
GC Determination of Pentachlorophenol in Aquatic Products
摘 要
水产品经正己烷提取,再经浓硫酸净化,用于消除色素等杂质的干扰和碳酸钾反萃取时严重的乳化现象;最后经乙酸酐衍生后用于气相色谱法测定其中五氯酚含量.五氯酚的质量浓度在100 μg·L-1以内与其峰面积呈线性关系.方法用于水产品分析,相对标准偏差(n=6)为3.0%~6.2%,回收率在85.0%~102.0%之间.
气相色谱法
水产品
Pentachlorophenol
GC
Aquatic products
Abstract
A method of GC for the determination of pentachlorophenol in aquatic products was proposed.The sample of aquatic product was extracted with n-hexane,and the extract obtained was treated with conc.H2SO4 to eliminate interferences of those coloring impurities and the appearance of emulsification in the process of back extraction with potassium carbonate solution.The pentachlorophenol in the K2CO3 solution was then derivatized with acetic anhydride,and the derivatized product was determined by GC.Linear relationship between values of peak area and mass concentration of pentachlorophenol was kept in the range within 100 μg·L-1.The proposed method was applied to the analysis of aquatic products,giving values of recovery and RSD′s (n=6) in the ranges of 85.0%-102.0% and 3.0%-6.2%,respectively.
中图分类号 O657.7
所属栏目 试验与研究
基金项目 海洋公益性行业科研专项经费项目(200805031)
收稿日期 2009/6/18
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备注张世娟(1981-),女,山东日照人,硕士,主要从事水产品质量安全研究.
引用该论文: ZHANG Shi-juan,XU Ying-jiang,GONG Xiang-hong,ZHANG Xiu-zhen,DENG Xu-xiu. GC Determination of Pentachlorophenol in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(9): 996～999
张世娟,徐英江,宫向红,张秀珍,邓旭修. 气相色谱法测定水产品中五氯酚[J]. 理化检验－化学分册, 2010, 46(9): 996～999
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参考文献
【1】江焘.法医毒物分析[M].2版.北京:人民卫生出版社,1998:138．
【2】KEITH L H,TELLIARD W A.ES & T special report: priority pollutants: I-a perspective view[J].Environ Sci Technol,1979,13(4):416-423．
【3】JAUREGUI O,GALCERAN M T.Determination of phenols in water by on-line solid-phase disk extraction and liquid chromatography with electrochemical detection[J].Anal Chim Acta,1997,340:191-199．
【4】李小敏,何佶.固相萃取-高效液相色谱法测定水中酚同系物[J].理化检验-化学分册,2008,44(11):1105-1107．
【5】黄卫红,李春香,柳天舒,等.同时亚临界水萃取与固相萃取从河流沉积物中分离有机氯化合物[J].理化检验-化学分册,2007,43(11):950-955．
【6】胡小钟,余建新,林雁飞,等.串联质谱法快速分析皮革中五氯酚残留[J].分析化学,2000,28(6):727-730．
【7】CRESPIN M A,GALLEGO M,VALCARCEL M S.Solid-phase extraction method for the determination of free and conjugated phenol compounds in human urine[J].J Chromatogr B,2002,773(2):89-96．
【8】孙磊,蒋新,周健民,等.红壤中痕量五氯酚的气相色谱法测定[J].分析化学,2003,31(6):716-719．
【9】肖宇芳,刘广民,董永亮,等.土壤中五氯酚的快速测定[J].岩矿测试,2008,27(2):117-119．
【10】MARTINEZ V J L,BELMONTE V A,GARRIDO F A,et al.Determination of fifteen priority phenolic compounds in environmental samples from Andalusia (Spain) by liquid chromatography-mass spectrometry[J].Anal Bioanal Chem,2004,379:125-130．
【11】费志良,葛家春,吴军,等.气相色谱测定青虾、草鱼肌肉中五氯苯酚及其钠盐残留总量的方法[J].南京师大学报:自然科学版,2004,27(3):70-73．
【12】李继革,戚双祥,周凯.双壳类水产品中微量五氯酚的气相色谱法测定[J].中国卫生检验杂志,2004,14(6):718-719．
【2】KEITH L H,TELLIARD W A.ES & T special report: priority pollutants: I-a perspective view[J].Environ Sci Technol,1979,13(4):416-423．
【3】JAUREGUI O,GALCERAN M T.Determination of phenols in water by on-line solid-phase disk extraction and liquid chromatography with electrochemical detection[J].Anal Chim Acta,1997,340:191-199．
【4】李小敏,何佶.固相萃取-高效液相色谱法测定水中酚同系物[J].理化检验-化学分册,2008,44(11):1105-1107．
【5】黄卫红,李春香,柳天舒,等.同时亚临界水萃取与固相萃取从河流沉积物中分离有机氯化合物[J].理化检验-化学分册,2007,43(11):950-955．
【6】胡小钟,余建新,林雁飞,等.串联质谱法快速分析皮革中五氯酚残留[J].分析化学,2000,28(6):727-730．
【7】CRESPIN M A,GALLEGO M,VALCARCEL M S.Solid-phase extraction method for the determination of free and conjugated phenol compounds in human urine[J].J Chromatogr B,2002,773(2):89-96．
【8】孙磊,蒋新,周健民,等.红壤中痕量五氯酚的气相色谱法测定[J].分析化学,2003,31(6):716-719．
【9】肖宇芳,刘广民,董永亮,等.土壤中五氯酚的快速测定[J].岩矿测试,2008,27(2):117-119．
【10】MARTINEZ V J L,BELMONTE V A,GARRIDO F A,et al.Determination of fifteen priority phenolic compounds in environmental samples from Andalusia (Spain) by liquid chromatography-mass spectrometry[J].Anal Bioanal Chem,2004,379:125-130．
【11】费志良,葛家春,吴军,等.气相色谱测定青虾、草鱼肌肉中五氯苯酚及其钠盐残留总量的方法[J].南京师大学报:自然科学版,2004,27(3):70-73．
【12】李继革,戚双祥,周凯.双壳类水产品中微量五氯酚的气相色谱法测定[J].中国卫生检验杂志,2004,14(6):718-719．
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