HPLC Determination of Phenols in Water with Solid Phase Extraction
摘 要
水样中7种酚同系物用固相萃取法在Oasis HLB柱上预富集,经吹氮干燥后用1 mL甲醇将包括苯酚、4-硝基酚、3-甲基酚、2-氯酚、2,4-二氯酚、2,4,6-三氯酚及五氯酚在内的7种酚同系物从柱上淋洗,所得淋出液直接进样进行高效液相色谱法测定.在所提出的最佳测定条件下,4-硝基酚质量浓度在4.0 mg·L-1以内,其余6种酚同系物质量浓度在20.0 mg·L-1以内与相应的检测信号之间呈线性关系,以10倍信噪比计算方法的测定下限,测得4-硝基酚的测定下限为0.02 mg·L-1,其余6种酚同系物为0.1 mg·L-1以下.用标准加入法测定方法的回收率,所用基体水样中未检出上述7种酚同系物,测得回收率在79.4%~103.0%之间,相应的相对标准偏差(n=7)在1.0%~6.7%之间.
Abstract
Seven phenol homologues in water sample were enriched by solid phase extraction (SPE) on the Oasis HLB column.After drying by N2-blowing,phenols (including phenol,4-nitrophenol,3-methyl phenol,2-chlorophenol,2,4-dichlorophenol,2,4,6-trichlorophenol,and pent chlorophenol) were eluted from the column with 1 mL of methanol,which was introduced into the instrument and determined by HPLC.Under the optimum condition of determination,linear relationships between values of analytical signals and concentration of the phenols were obtained in the range within 4.0 mg·L-1 for 4-nitrophenol,and in ranges within 20.0 mg·L-1 for the remainders.Lower limits of determination (10S/N) found for 4-nitrophenol was 0.02 mg·L-1,and for the remainder were less than 0.1 mg·L-1.Tests for recovery of the method were made by addition of standard solutions of the 7 phenol homologues to water samples in which phenols were not detected,values of recovery obtained were in the range of 79.4% to 103.0%,with values of RSD′s (n=7) in the range of 1.0%-6.7%.
中图分类号 O657.37
所属栏目 工作简报
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收稿日期 2007/7/4
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备注李小敏(1978- ),女,浙江永康人,硕士,主要从事水质检测分析工作.
引用该论文: LI Xiao-min,HE Ji. HPLC Determination of Phenols in Water with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(11): 1105~1107
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
被引情况:
【1】刘静,曾兴宇,烟卫, "顶空固相微萃取-气相色谱法测定饮用水中氯酚",理化检验-化学分册 47, 921-923(2011)
【2】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",理化检验-化学分册 46, 996-999(2010)
【3】易谷洋,魏瑞萍,谭小旺,宋燕西, "多壁碳纳米管固相萃取-高效液相色谱法测定水中四溴双酚A",理化检验-化学分册 49, 487-488(2013)
【4】叶存玲,刘清玲,谢国红,王治科, "分散液相微萃取-高效液相色谱法测定水样中扑虱灵和哒螨灵",理化检验-化学分册 47, 1391-1394(2011)
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参考文献
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【4】Sarrion M N,Santos F J,Galceran M T.Determination of chlorophenols by solid-phase microextraction and liquid chromatography with electrochemical detection[J].Journal of Chromatography A,2002,947(2):155-165.
【5】Korenman Y I,Gruzdev I V,Kondratenok B M,et al.Determination of chlorophenols in potable water: preconcentration by solvent extraction,derivatization of the extract,and chromatographic analysis of the derivatives[J].Journal of Analytical Chemistry,2003,58(7):635.
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