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采用顶空固相微萃取改进丙二醛测定法及其在植物化学物抗氧化活性测定中的应用

Improved malonaldehyde assay using headspace solid-phase microextraction and its application to the measurement of the antioxidant activity of phytochemicals.

作者信息

Fujioka Kazutoshi, Shibamoto Takayuki

机构信息

Department of Environmental Toxicology, University of California, One Shields Avenue, Davis, California 95616, USA.

出版信息

J Agric Food Chem. 2005 Jun 15;53(12):4708-13. doi: 10.1021/jf050297q.

DOI:10.1021/jf050297q
PMID:15941304
Abstract

A modified malonaldehyde (MA) assay for antioxidant activity, which involves derivatization and headspace solid-phase microextraction (HS-SPME) was developed and validated. The recovery of MA as 1-methylpyrazole (product of MA and N-methylhydrazine) from a headspace of an aqueous solution containing MA, buffer, surfactant, and cod liver oil using HS-SPME with a PDMS/DVB fiber was 91.3 +/- 3.38%. MA was analyzed by a gas chromatograph with a nitrogen-phosphorus detector, and its detection limit was 0.0103 nmol/mL. The antioxidant activities of natural compounds were determined as the percentage inhibition of MA formed from cod liver oil oxidized by Fenton's reagents in the above aqueous solution. Sesamol inhibited MA formation most (86.1%), followed by eugenol (84.4%), capsaicin (80.7%), ethylvanillin (45.3%), and vanillin (31.6%) at a level of 50 microg/mL. This method did not require any organic solvents and is a simple, fast, and a highly sensitive method for MA determination.

摘要

开发并验证了一种用于抗氧化活性的改良丙二醛(MA)测定方法,该方法涉及衍生化和顶空固相微萃取(HS-SPME)。使用带有PDMS/DVB纤维的HS-SPME从含有MA、缓冲液、表面活性剂和鱼肝油的水溶液顶空中回收作为1-甲基吡唑(MA与N-甲基肼的产物)的MA,回收率为91.3±3.38%。通过带有氮磷检测器的气相色谱仪分析MA,其检测限为0.0103 nmol/mL。天然化合物的抗氧化活性通过上述水溶液中由芬顿试剂氧化鱼肝油形成的MA的抑制百分比来确定。在50μg/mL的水平下,芝麻酚对MA形成的抑制作用最大(86.1%),其次是丁香酚(84.4%)、辣椒素(80.7%)、乙基香兰素(45.3%)和香兰素(31.6%)。该方法不需要任何有机溶剂,是一种简单、快速且高度灵敏的MA测定方法。

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