响应面试验优化溶剂诱导萃取水系基质中棒曲霉素工艺及其检测分析

Optimization of Solvent Induced Phase Transition Extraction of Patulin from Aqueous Matrix by Response Surface Methodology for HPLC Analysis

基于溶剂诱导萃取,使用响应面法优化水系基质中棒曲霉的提取工艺,并对4种不同水系基质的料液比(V/V)进行选择。在单因素试验基础上,以棒曲霉素转移率为指标,响应面法优化溶剂诱导萃取的条件,并在不同料液比的4种水系基质中进行加标回收实验。通过溶剂诱导分层,获得棒曲霉素的最佳萃取条件为乙腈-样品体积比7∶3、Na Cl添加量1.4?g/3 m L样品、提取温度34℃,此条件下,棒曲霉素转移率为90.47%。在此最优条件下,苹果基质的最优料液比为7∶3,浓缩苹果汁、酿酒葡萄和葡萄酒基质的最优料液比均为1∶9,加标回收率分别为91.08%、85.51%、88.74%、89.17%。同时与中华人民共和国出入境检验检疫行业标准SN/T 2008—2007《进出口果汁中棒曲霉毒素的检测方法高效液相色谱法》进行比较,结果显示该前处理方法溶剂使用量少、操作简单且重复性好。综上,响应面法优化溶剂诱导分相萃取棒曲霉素的结果可靠,为水系基质中棒曲霉素的萃取提供了一种全新、快速的前处理方法。

Response surface methodology was adopted to optimize the extraction of patulin from an aqueous matrix.Meanwhile,the optimal solid-to-liquid ratios(V/V)for four different aqueous matrixes were selected.Optimization ofthe extraction conditions for improved recovery of patulin was done by the combined use of one-factor-at-a-time methodand response surface methodology.Recovery experiments were conducted with spiked samples at solid-to-liquid ratiosusing four different aqueous matrixes.The optimal extraction conditions established were as follows:acetonitrile toaqueous sample ratio,7:3;NaCl dosage,1.4g/3mL sample;and extraction temperature,34℃.Under these conditions,the recovery of patulin was90.47%,and the optimal solid-to-liquid ratios were7:3for apple pulp matrix and1:9forconcentrated apple juice,wine grape and wine,giving a recovery of91.08%,85.51%,88.74%and89.17%from spikedsamples,respectively.At the same time,over the entry-exit inspection and quarantine industry standard method(SN/T2008-2007),the pre-treatment method was advantageous in terms of less solvent consumption,simple operationand good reproducibility.Collectively,we concluded that the solvent induced phase transition extraction of patulinoptimized by response surface methodology yielded reliable predictions and it had the potential to provide a new pretreatmentmethod for the extraction of patulin from aqueous matrices.