基质固相分散-气相色谱质谱联用法测定沉香中精油的化学成分  

Matrix Solid-phase Dispersion Combined with GC-MS for Determination of Chemical Constituents of Essential Oil in Agarwood

作　　者：陈虹霞[1] 周昊[1,2] 叶建中[1] 陶冉[1] 李文君[1] 王成章[1,2] CHEN Hongxia;ZHOU Hao;YE Jianzhong;TAO Ran;LI Wenjun;WANG Chengzhang(Institute of Chemical Industry of Forest Products,CAF,National Engineering Lab. for Biomass Chemical Utilization,Key Lab. of Chemical Engineering of Forest Products,National Forestry and Grassland Administration,Key Lab. of Biomass Energy and Material,Jiangsu Province,Jiangsu Co-Innovation Center for Efficient Processing and Utilization of Forest Resources,Nanjing 210042,China;Research Institute of Forestry New Technology,CAF,Beijing 100091,China)

机构地区：[1]中国林业科学研究院林产化学工业研究所,生物质化学利用国家工程实验室,国家林业和草原局林产化学工程重点实验室,江苏省生物质能源与材料重点实验室,江苏省林业资源高效加工利用协同创新中心,江苏南京210042 [2]中国林业科学研究院林业新技术研究所,北京100091

出　　处：《林产化学与工业》2021年第3期47-54,共8页Chemistry and Industry of Forest Products

基　　金：中国林科院中央级公益性科研院所基本科研业务费专项资金(CAFYBB2018GA001);中国林科院林产化学工业研究所研究团队建设创新工程项目(LHSXKQ5)。

摘　　要：以海南生物结香的沉香木为原料,建立了沉香精油的基质固相分散-气相色谱/质谱联用(MSPD-GC/MS)分析方法。采用基质固相分散技术进行沉香精油的提取,采用单因素试验得到优化工艺条件为:吸附基质为硅酸镁,吸附基质与样品的质量比为4∶1,分散溶剂为异丙醇,分散溶剂与样品的比例为4∶1(mL∶g),洗脱溶剂为体积比9∶1的正己烷和乙酸乙酯混合液,洗脱溶剂用量6 mL,在此条件下,沉香精油的提取得率为(9.19±0.15)%,明显高于乙醚超声波提取方法的(6.65±0.22)%。采用GC/MS分析沉香精油成分,并与乙醚超声波提取方法进行比较。基质固相分散提取的沉香精油成分组成与乙醚超声波提取相似,主要为2.13%的芳香族类、25.67%的倍半萜类、26.85%的色酮类和7.5%的脂肪族。相比乙醚超声波提取,基质固相分散提取的沉香精油中倍半萜类化合物的成分更多,主要有γ-芹子烯、β-檀香醇、缬草-4,7(11)二烯、α-愈创木烯、白菖醇和1,9-马兜铃二烯。MSPD-GC/MS分析方法能够真实地反映沉香精油的化学成分,可作为沉香品质评价的一种快速鉴别方法。Matrix solid-phase dispersion-gas chromatography combined with mass spectrometry(MSPD-GC/MS)analysis method for essential oil was established based on Hainan agarwood induced by biotechnological method.The MSPD conditions of extracting agarwood essential oil established by single factor test were magnesium silicate as the adsorbent,adsorbent/sample mass ratio 4∶1,isopropanol as the dispersion solvent,dispersion solvent/sample ratio 4∶1(mL∶g)and 6 mL n-hexane/ethyl acetate 9∶1(volume ratio)as the elution solvent.Under these conditions,the extraction yield of MSPD was(9.19±0.15)%,which was higher than ultrasonic assisted ether extraction(6.65±0.22)%.The chemical constituents of essential oil were analysis by GC/MS,and compared with that extracted by ultrasonic assisted ether extraction.The compositions of essential oil extracted by MSPD were similar to ultrasonic assisted ether extraction,the main constituents were 2.13%aromatic,25.67%sesquiterpenoids,26.85%chromones and 7.50%aliphatic compounds.The number of sesquiterpenoids in the essential oil extracted by MSPD was more than that of ultrasonic assisted ether extraction,such asγ-selinene,β-santalol,valerena-4,7(11)-diene,α-guaiene,shyobunol and 1,9-aristo-ladiene.Thus,the MSPD-GC/MS analysis method could truly reflect the chemical composition of agarwood essential oil,which could be used as a rapid identification method for the quality evaluation of agarwood.

关 键 词：沉香 精油 基质固相分散 气质联用 化学成分 

分 类 号：TQ35[化学工程]