School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.
School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.
Talanta. 2014 Mar;120:47-54. doi: 10.1016/j.talanta.2013.11.081. Epub 2013 Dec 4.
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).
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。