基于HS-GC-MS考察樟帮特色米泔水漂法对白术与麸炒白术挥发性成分的影响

Analysis of Effect of Characteristic Processing with Rice-washed Water on Volatile Components in Raw and Bran-fried Products of Atractylodis Macrocephalae Rhizoma by HS-GC-MS

目的:通过比较白术与漂白术、麸炒白术与麸炒漂白术挥发性成分组成和含量差异,考察樟帮特色米泔水漂法对白术及其麸炒品挥发性成分的影响。方法:采用顶空气相色谱-质谱法(HS-GC-MS)检测白术生品、麸炒品及二者米泔水制品的挥发性成分,GC条件为程序升温(起始柱温50℃,以10℃·min^(-1)升至140℃,维持5 min;以4℃·min^(-1)升至210℃),分流比10∶1,载气为高纯氦气,溶剂延迟时间3 min;MS条件为电子轰击离子源(EI),电子碰撞能量70 eV,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软件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),根据变量重要性投影(VIP)值>1和P<0.05筛选得到白术与漂白术、麸炒白术与麸炒漂白术的差异性成分。结果:共鉴定出71种挥发性成分,其中白术53种、漂白术50种、麸炒白术51种、麸炒漂白术44种。OPLS-DA结果表明白术与漂白术、麸炒白术与麸炒漂白术之间存在明显差异,但不同产地间白术样品的差异不明显。白术与漂白术、麸炒白术与麸炒漂白术比较,化合物组成变化较小,但单萜类及倍半萜成分的含量变化较大。结论:白术与漂白术、麸炒白术与麸炒漂白术挥发性成分含量发生了显著变化,其中1,2-dimethyl-4-methylidenecyclopentene、γ-榄香烯、姜烯、9,10-dehydro-isolongifolene、苍术酮、silphinene、modhephene和(1S,4S,4a S)-1-isopropyl-4,7-dimethyl-1,2,3,4,4a,5-hexahydronaphthalene等成分可作为白术米泔水漂制前后挥发性成分候选差异性标志物。

Objective:By comparing the differences in composition and content of volatile components between Atractylodis Macrocephalae Rhizoma(AMR)and bleaching AMR,bran-fried AMR and bran-fried bleaching AMR,the effect of processing with rice-washed water on the volatile components in AMR and bran-fried AMR were investigated.Method:Headspace gas chromatography-mass spectrometry(HS-GC-MS)was used to determine the volatile components in raw products,bran-fried products and their processed products with rice-washed water.GC conditions were programmed temperature(starting temperature of 50℃,rising to 140℃at 10℃·min^(-1),maintained for 5 min,then rising to 210℃at 4℃·min^(-1)),splitting ratio of 10∶1,high purity helium as the carrier gas and a solvent delay time of 3 min.MS conditions were an electron bombardment ion source(EI)with an electron collision energy of 70 eV,ion source temperature of 230℃,and the detection range of m/z 20-650.The relative contents of the components were determined by the peak area normalization method,the obtained sample data were subjected to principal component analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLS-DA)by SIMCA 14.1 software,and the differential components of AMR and bleaching AMR,and bran-fried AMR and bran-fried bleaching AMR were screened according to variable importance in the projection(VIP)value>1 and P<0.05.Result:A total of 71 volatile components were identified,including 53 in AMR,50 in bleaching AMR,51 in bran-fried AMR,and 44 in bran-fried bleaching AMR.OPLS-DA results showed that there were significant differences between AMR and bleaching AMR,bran-fried AMR and bran-fried bleaching AMR,but not between AMR samples from different origins.The compound composition of AMR and bleaching AMR,bran-fried AMR and bran-fried bleaching AMR did not change,but the contents of monoterpenes and sesquiterpenes changed significantly.Conclusion:Significant changes in the contents of volatile components were observed in AMR and bleaching AMR,bran-fried AMR and bran-fried bleaching AMR,among them,1,2-dimethyl-4-methylidenecyclopentene,9,10-dehydro-isolongifolene,γ-elemene,zingiberene,atractylone,silphinene,modhephene and(1S,4S,4a S)-1-isopropyl-4,7-dimethyl-1,2,3,4,4a,5-hexahydronaphthalene can be used as candidate differential markers of volatile components of AMR before and after processing with rice-washed water.