食品科学 ›› 2017, Vol. 38 ›› Issue (6): 215-220.doi: 10.7506/spkx1002-6630-201706034

• 工艺技术 • 上一篇    下一篇

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

陈 霞,王 波,叶 融,李 敏,周继亘,张 波,韩舜愈   

  1. 1.甘肃农业大学食品科学与工程学院,甘肃省葡萄与葡萄酒工程学重点实验室,甘肃 兰州 730070;2.甘肃出入境检验检疫局综合技术中心,甘肃 兰州 730000;3.北京林业大学生物科学与技术学院,北京 100083
  • 出版日期:2017-03-25 发布日期:2017-03-28
  • 基金资助:
    国家自然科学基金地区科学基金项目(31160310)

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

CHEN Xia, WANG Bo, YE Rong, LI Min, ZHOU Jigen, ZHANG Bo, HAN Shunyu   

  1. 1. Key Laboratory of Viticulture and Oenology of Gansu Province, College of Food Science and Engineering, Gansu Agricultural University, Lanzhou 730070, China; 2. Central Laboratory of Technical Center of Gansu Entry-Exit Inspection and Quarantine Bureau, Lanzhou 730000, China; 3. College of Biological Sciences and Technology, Beijing Forestry University, Beijing 100083, China
  • Online:2017-03-25 Published:2017-03-28

摘要: 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、NaCl添加量1.4 g/3 mL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。

关键词: 高效液相色谱, 响应面, 棒曲霉素, 水系基质, 溶剂诱导萃取

Abstract: 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 of the extraction conditions for improved recovery of patulin was done by the combined use of one-factor-at-a-time method and response surface methodology. Recovery experiments were conducted with spiked samples at solid-to-liquid ratios using four different aqueous matrixes. The optimal extraction conditions established were as follows: acetonitrile to aqueous sample ratio, 7:3; NaCl dosage, 1.4 g/3 mL sample; and extraction temperature, 34 ℃. Under these conditions, the recovery of patulin was 90.47%, and the optimal solid-to-liquid ratios were 7:3 for apple pulp matrix and 1:9 for concentrated apple juice, wine grape and wine, giving a recovery of 91.08%, 85.51%, 88.74% and 89.17% from spiked samples, respectively. At the same time, over the entry-exit inspection and quarantine industry standard method (SN/T 2008-2007), the pre-treatment method was advantageous in terms of less solvent consumption, simple operation and good reproducibility. Collectively, we concluded that the solvent induced phase transition extraction of patulin optimized by response surface methodology yielded reliable predictions and it had the potential to provide a new pretreatment method for the extraction of patulin from aqueous matrices.

Key words: high performance liquid chromatography (HPLC), response surface methodology, patulin, aqueous matrix, solvent induced phase transition extraction

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