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涡旋辅助液液微萃取结合高效液相色谱法测定果汁中的糠醛和棒曲霉素。

Vortex-assisted liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of furfurals and patulin in fruit juices.

机构信息

School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.

School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.

出版信息

Talanta. 2014 Mar;120:47-54. doi: 10.1016/j.talanta.2013.11.081. Epub 2013 Dec 4.

DOI:10.1016/j.talanta.2013.11.081
PMID:24468341
Abstract

A fast and simple solvent microextraction technique using salting out-vortex-assisted liquid-liquid microextraction (salting out-VALLME) was developed for the extraction of furfurals (2-furfural (2-F), 3-furfural (3-F), 5-methylfurfural (5-MF) and 5-hydroxymethylfurfural (5-HMF)) and patulin (PAT) in fruit juice samples. The optimum extraction conditions for 5 mL sample were: extraction solvent, 1-hexanol; volume of extractant, 200 µL; vortex time, 45 s; salt addition, 20%. The simultaneous determination of the furfurals and PAT were investigated using high performance liquid chromatography coupled with diode array detector (HPLC-DAD). The separation was performed using ODS Hypersil C18 column (4.6 mm i.d × 250 mm, 5 μm) under gradient elution. The detection wavelengths used for all compounds were 280 nm except for 3-F (210 nm). The furfurals and PAT were successfully separated in less than 9 min. Good linearities (r(2)>0.99) were obtained within the range 1-5000 μg L(-1) for all compounds except for 3-F (10-5000 µg L(-1)) and PAT (0.5-100 μg L(-1)). The limits of detection (0.28-3.2 µg L(-1)) were estimated at S/N ratio of 3. The validated salting out-VALLME-HPLC method was applied for the analysis of furfurals and PAT in fruit juice samples (apple, mango and grape).

摘要

一种快速简便的溶剂微萃取技术,采用盐析-涡旋辅助液-液微萃取(salting out-VALLME),用于从果汁样品中提取糠醛(2-糠醛(2-F)、3-糠醛(3-F)、5-甲基糠醛(5-MF)和 5-羟甲基糠醛(5-HMF))和棒曲霉素(PAT)。对于 5 mL 样品,最佳萃取条件为:萃取溶剂,1-己醇;萃取剂体积,200 μL;涡旋时间,45 s;加盐量,20%。采用高效液相色谱-二极管阵列检测器(HPLC-DAD)同时测定糠醛和 PAT。采用 ODS Hypersil C18 柱(4.6 mm i.d×250 mm,5 μm)在梯度洗脱下进行分离。所有化合物的检测波长均为 280 nm,除 3-F(210 nm)外。糠醛和 PAT 在不到 9 分钟内得到很好的分离。所有化合物在 1-5000 μg L(-1)范围内均具有良好的线性(r(2)>0.99),除 3-F(10-5000 µg L(-1))和 PAT(0.5-100 μg L(-1))外。检测限(0.28-3.2 µg L(-1))在信噪比为 3 时估算。经验证的盐析-涡旋辅助液-液微萃取-HPLC 方法用于分析果汁样品(苹果、芒果和葡萄)中的糠醛和 PAT。

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