基于HS-GC-MS考察苍术米泔水漂制前后挥发性成分的变化

Analysis of Differences of Volatile Components in Atractylodis Rhizoma Before and After Processing with Rice-washed Water by HS-GC-MS

目的通过比较苍术经米泔水漂制前后的挥发性成分组成与含量变化,考察米泔水炮制对苍术挥发性成分的影响。方法采用顶空气相色谱-质谱法(HS-GC-MS)检测北苍术、茅苍术及二者米泔水制品的挥发性成分,色谱条件采用程序升温(起始柱温50℃,维持2 min;以10℃·min^(-1)升温至120℃,以2.5℃·min^(-1)升温至170℃,以10℃·min^(-1)升温至240℃,维持3 min),进样口温度280℃,分流比为10∶1,溶剂延迟时间3 min;质谱条件为电子轰击离子源(EI),离子源温度230℃,扫描范围m/z 20~650,采用峰面积归一化法测定各成分的相对质量分数。运用SIMCA 14.1对所得样品数据进行主成分分析(PCA)及正交偏最小二乘法-判别分析(OPLS-DA),通过变量重要性投影(VIP)值>1的原则筛选北苍术、茅苍术与其炮制品的差异性成分。结果共鉴定出60种化合物,其中北苍术40种、制北苍术38种、茅苍术46种、制茅苍术47种。PCA及OPLS-DA均显示,4种苍术样品各自聚为一类,表明2种苍术经米泔水炮制后挥发性成分均发生明显变化,且北苍术和茅苍术的挥发性成分差异明显。2种苍术的生品与其炮制品比较,化合物组成基本不变,但含量有明显变化,差异性成分主要聚集在单萜类及倍半萜类化合物,且单萜类化合物含量多呈下降趋势。结论北苍术、茅苍术经米泔水炮制后挥发性成分的含量发生了明显变化,蒎烯、3-蒈烯、4-异丙基甲苯、罗勒烯、萜品油烯、苍术酮、乙酸、糠醛可作为炮制前后的差异性标志物。

Objective By comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water,the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated.Method Headspace-gas chromatography-mass spectrometry(HS-GC-MS)was used to detect the volatile components in rhizomes of Atractylodes chinensis and A.lancea,and their processed products of rice-washed water.Chromatographic conditions were programmed temperature(starting temperature of 50℃for 2 min,rising to 120℃with the speed of 10℃·min^(-1),then rising to 170℃at 2.5℃·min^(-1),and rising to 240℃at 10℃·min^(-1) for 3 min),the inlet temperature was 280℃,the split ratio was 10∶1,and the solvent delay time was 3 min.The conditions of mass spectrometry were electron bombardment ionization(EI)with ionization temperature at 230℃and detection range of m/z 20-650.Then the relative content of each component was determined by the peak area normalization method.SIMCA 14.1 software was used to perform unsupervised principal component analysis(PCA)and supervised orthogonal partial least squares-discriminant analysis(OPLS-DA)on each sample data,the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection(VIP)value>1.Result A total of 60 components were identified,among which 40 were rhizomes of A.chinensis and 38 were its processed products,46 were rhizomes of A.lancea and 47 were its processed products.PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively,indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water,and there were also significant differences in the volatile components of rhizomes of A.lancea and A.chinensis.The compound composition of Atractylodis Rhizoma and its processed products was basically the same,but the content of the compounds was significantly different.The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids,and the content of monoterpenoids mostly showed a decreasing trend.Conclusion After processing with rice-washed water,the contents of volatile components in rhizomes of A.lancea and A.chinensis are significantly changed,and pinene,3-carene,p-cymene,ocimene,terpinolene,atractylon,acetic acid and furfural can be used as difference markers before and after processing.