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用于测定生物油中低分子量醛的色谱方法。

Chromatographic approaches for determination of low-molecular mass aldehydes in bio-oil.

机构信息

Departamento de Análisis Instrumental, Facultad de Farmacia, Universidad de Concepción, Concepción, Chile.

出版信息

J Chromatogr A. 2012 Jan 6;1219:154-60. doi: 10.1016/j.chroma.2011.10.093. Epub 2011 Nov 7.

Abstract

HPLC-UV and GC/MS determination of aldehydes in bio-oil were evaluated. HPLC-UV preceded by derivatization with 2,4-dinitrophenylhydrazine allows separation and detection of bio-oil aldehydes, but the derivatization affected the bio-oil stability reducing their quantitative applicability. GC/MS determination of aldehydes was reached by derivatization with o-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride. Two approaches for this reaction were evaluated. The first: "in solution derivatization and head space extraction" and the second: "on fiber derivatization SPME", the latter through an automatic procedure. Both sample treatments allows the quantification of most important aliphatic aldehydes in bio-oil, being the SPME approach more efficient. The aldehyde concentrations in bio-oil were ~2% formaldehyde, ~!0.1% acetaldehyde and ~0.05% propionaldehyde.

摘要

采用高效液相色谱-紫外(HPLC-UV)和气相色谱/质谱联用(GC/MS)法测定生物油中的醛类物质。采用 2,4-二硝基苯肼衍生化法对生物油中的醛类物质进行 HPLC-UV 分析,可以对其进行分离和检测,但衍生化会影响生物油的稳定性,降低其定量适用性。采用邻-(2,3,4,5,6-五氟苄基)羟胺盐酸盐衍生化法对醛类物质进行 GC/MS 分析。评估了两种衍生化方法:第一种是“溶液衍生化和顶空萃取”,第二种是“纤维上衍生化 SPME”,后者通过自动程序进行。这两种样品处理方法均能定量测定生物油中大多数重要的脂肪族醛类物质,其中 SPME 方法更为有效。生物油中的醛类浓度约为 2%的甲醛、0.1%的乙醛和0.05%的丙醛。

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