Optimization of the HS-SPME-GC-MS Technique for Determination of Volatile Flavor Compounds in Pork by Response Surface Methodology
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摘要: 本试验采用顶空固相微萃取-气相色谱-质谱技术(Headspace solid phase microextraction-gas chromatography-mass spectrometry,HS-SPME-GC-MS)检测猪肉经过热处理后的挥发性风味物质。以盐度、萃取时间、萃取温度和解吸时间为影响因素进行单因素实验,采用响应面法对萃取条件进行优化,并在此基础上分析其挥发性风味物质的组成。结果表明:各因素的影响强弱顺序为:盐度>萃取温度>萃取时间>解吸时间。采用75 μm碳分子筛/聚二甲基硅氧烷(Carbon/Polydimethylsiloxane,CAR/PDMS)萃取头,最佳萃取条件为盐度6%,萃取温度为73℃、萃取时间为40 min、解吸时间为3 min。在此条件下,猪肉共检测出醛类、醇类、烃类、酮类、酯类、酸类、含硫及其它杂环化合物等38种挥发性风味物质,总峰面积为3.18×1010,综合得分为99.71分,验证试验结果与预测值的相对误差为0.27%,模型拟合度好。研究结果可为猪肉挥发性风味物质的分析和调控提供一定的理论依据。
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关键词:
- 顶空固相微萃取(HS-SPME) /
- 气相色谱-质谱(GC-MS) /
- 猪肉 /
- 挥发性风味物质 /
- 响应面法
Abstract: In this study, the headspace solid phase microextraction-gas chromatography-mass spectrometry(HS-SPME-GC-MS) was used to detect the volatile flavor compounds of heating treatment on pork. The influencing factors such as salinity, extraction time, extraction temperature and desorption time were researched by single factor experiment, and the extraction conditions were optimized by response surface methodology. On this basis, the composition of volatile flavor compounds was analyzed. The results showed the order of influence of four factors was as follows: salinity>extraction temperature>extraction time>desorption time. The 75 μm carbon/polydimethylsiloxane(CAR/PDMS) fiber was used and the optimum extraction conditions of pork were as follows: the salinity was 6%, extraction temperature was 73℃, extraction time was 40 min and desorption time was 3 min. Under these conditions, there were 38 kinds of main volatile flavor compounds were detected in pork, including aldehydes, alcohols, hydrocarbons, ketones, esters, acids and sulfur heterocyclics, etc. The total peak area was 3.18×1010, and the comprehensive score was 99.71 with a deviation of 0.27% from the predicted value, the model fitted well. The results of study could provide some theoretical basis for the analysis and regulation of volatile flavor compounds in pork. -
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