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固相萃取-高效液相色谱-二极管阵列检测法测定苹果 cider 和葡萄酒中呋喃衍生物

An efficient method for the determination of furan derivatives in apple cider and wine by solid phase extraction and high performance liquid chromatography--diode array detector.

机构信息

Guelph Food Research Centre, Agriculture and Agri-Food Canada, Guelph, ON, Canada.

出版信息

J Chromatogr A. 2013 Apr 5;1284:100-6. doi: 10.1016/j.chroma.2013.02.002. Epub 2013 Feb 8.

DOI:10.1016/j.chroma.2013.02.002
PMID:23452467
Abstract

A reliable SPE-HPLC/DAD method was developed for the simultaneous separation and quantitation of 10 furan derivatives in apple cider and wine matrices, including 5-hydroxymethyl-2-furaldehyde (5-HMFD), 4-hydroxy-2,5-dimethyl-3(2H)-furanone (4-HDMF), 2-furoic acid (2-FA), 2-furaldehyde (2-F), 3-furaldehyde (3-F), 2-acetylfuran (2-AF), 5-methyl-2-furaldehyde (5-MFD), methyl 2-furoate (MFT), 2-propionylfuran (2-PF) and ethyl 2-furoate (EFT). All the compounds were satisfactorily separated on a C18 column in less than 30 min. The solid phase extraction parameters have been optimized, including the sorbent, sample volume, washing and elution solvent. The relative standard deviations (RSDs) (intra- and inter-day) of all analytes were less than 6.4% for apple cider at 5mg/L spiking level and less than 3.9% (except 2-FA) for wine at 0.5mg/L spiking level. The limits of detection (LOD) and limits of quantitation (LOQ) were low (LOD 0.002-0.093 mg/L, LOQ 0.01-0.31 mg/L) compared to the usual concentrations of these compounds in these food matrices. The absolute recoveries of all compounds were higher than 77.8% (most of them were 80.5-103%) at different spiking levels (apple cider 0.5-50mg/L). The results showed that the developed method was precise, sensitive, robust and of good selectivity.

摘要

建立了一种可靠的 SPE-HPLC/DAD 方法,用于同时分离和定量苹果 cider 和葡萄酒基质中的 10 种呋喃衍生物,包括 5-羟甲基-2-糠醛(5-HMFD)、4-羟基-2,5-二甲基-3(2H)-呋喃酮(4-HDMF)、2-糠酸(2-FA)、2-糠醛(2-F)、3-糠醛(3-F)、2-乙酰基呋喃(2-AF)、5-甲基-2-糠醛(5-MFD)、甲基 2-呋喃甲酯(MFT)、2-丙酰基呋喃(2-PF)和乙基 2-呋喃酯(EFT)。所有化合物在不到 30 分钟的时间内在 C18 柱上得到满意的分离。优化了固相萃取参数,包括吸附剂、样品体积、洗涤和洗脱溶剂。在苹果 cider 中 5mg/L 加标水平下,所有分析物的日内和日间相对标准偏差(RSD)均小于 6.4%,在葡萄酒中 0.5mg/L 加标水平下,除 2-FA 外,所有分析物的 RSD 均小于 3.9%。检测限(LOD)和定量限(LOQ)均较低(LOD 0.002-0.093mg/L,LOQ 0.01-0.31mg/L),与这些化合物在这些食品基质中的常见浓度相比。在不同加标水平(苹果 cider 0.5-50mg/L)下,所有化合物的绝对回收率均高于 77.8%(大多数为 80.5-103%)。结果表明,所建立的方法精确、灵敏、稳健且选择性好。

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