基于HS-SPME-GC-MS对五常稻花香米挥发性指纹图谱构建

Construction of volatile fingerprint of Wuchang rice based on HS-SPME-GC-MS

利用顶空固相微萃取技术(HS-SPME)结合气相色谱质谱联用仪(GC-MS)对五常稻花香米(五优稻4号)的挥发性成分进行定性、定量分析,建立挥发性成分指纹图谱,并利用方法学验证指纹图谱的重复性与精密性。结果表明:在恒定平衡温度条件下,最佳试验条件为萃取头材质50/30μm PDMS-DVB-CAR、样品量15 g、平衡时间40 min、萃取时间30 min、解吸温度230℃、解吸时间1.0 min;共检测出相对含量大于0.01%的挥发性有机化合物118种,占总挥发性成分的98.41%;以峰面积、总相对丰度、特征峰值为重复性验证指标,相对标准偏差均小于0.50%;通过皮尔逊相关系数法和夹角余弦法对特征峰相似度分析,结果均大于0.980,说明该方法具有较好的重复性和精密性。

Headspace solid phase microextraction(HS-SPME) combined with gas chromatography-mass spectrometry(GC-MS) was used to qualitatively and quantitatively analyze the volatile components of Wuchang rice(Wuyou rice No.4),establish the fingerprint of volatile components,and verify the repeatability and precision of the fingerprint with methodology.The results showed that under the condition of constant equilibrium temperature,the best test condition was 50/30 μm PDMS-DVB-CAR extraction head material,sample weight 15 g,equilibrium time 40 min,extraction time 30 min,desorption temperature 230 ℃,desorption time 1.0 min.A total of 118 volatile organic compounds with relative content greater than 0.01 % were detected,accounting for 98.41 % of the total volatile components.Taking peak area,total relative abundance and characteristic peak value as the repeatability verification indexes,the relative standard deviation was less than 0.50 %.Pearson correlation coefficient method and included angle cosine method were used to analyze the similarity of characteristic peaks,and the results were both greater than 0.980,indicating that the method has good repeatability and precision.