Chinese Journal of Chromatography

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Determination of six p-hydroxybenzoates in fruits and jams using solid-phase extraction-high performance liquid chromatography

CHEN Ai1, HE Qiaosang2, WANG Pingya1*, ZHOU Yong1, HUANG Li1, XU Zhenjian1, ZHAO Hua1, ZHANG Weiying1   

  1. 1.National Marine Food Quality Supervision and Testing Center, Zhoushan 316021, China; 2.Zhejiang Province Food Quality and Safety Test Center, Hangzhou 310013, China
  • Received:2009-07-16 Revised:2009-09-16 Online:2009-11-30 Published:1981-12-25
  • Contact: WANG Pingya

Abstract: A method was developed for the determination of 6 p-hydroxybenzoates (methyl p-hydroxybenzoate (MHB), ethyl p-hydroxybenzoate (EHB), isopropyl p-hydroxybenzoate (IPHB), propyl p-hydroxybenzoate (PHB), isobutyl p-hydroxybenzoate (IBHB) and butyl p-hydroxybenzoate (BHB)) in fruits and jams using the combination of solid-phase extraction and high performance liquid chromatography (SPE-HPLC). Two different extraction solutions and three different mobile phases were tested for p-hydroxybenzoates analysis, and finally ethanol was used as the extraction solvent and methanol-citric acid buffer was selected as the mobile phase. The sample was extracted, and purified by an Oasis HLB solid-phase extraction cartridge, then separated on a Symmetry-C18 column and detected at the wave length of 258 nm. The results showed that all the calibration graphs were linear in the concentration range of 0.1~20.0 mg/L (r=0.9999). The detection limits and quantification limits were 0.1 mg/kg (S/N=3) and 0.3 mg/kg (S/N=10) respectively for MHB, EHB, IPHB and PHB, 0.2 mg/kg (S/N=3) and 0.6 mg/kg (S/N=10) respectively for IBHB and BHB. The average recoveries were between 82.8% and 115.5% with the relative standard deviations (RSDs) of 0.2%~6.8%(n=6). The method is simple, rapid, sensitive and reproducible, and can be used for the routine analysis of the p-hydroxybenzoates in fruits and jams.

Key words: fruits, high performance liquid chromatography (HPLC), jams , p-hydroxybenzoates, solid phase extraction (SPE)