生白术和炒白术挥发油成分的GC-MS分析

目的: 研究白术生品及其蜜炙麸皮炒制品挥发油的化学成分,比较二者之间的异同。 方法: 采用水蒸气蒸馏法分别提取生品白术、炒白术挥发油,计算挥发油得率并进行比较。气相色谱-质谱联用技术分析其成分,面积归一化法比较各组分间的相对含量。采用DB-5MS石英毛细管色谱柱(30 m×0.25 mm×0.25 μm),汽化温度270℃。程序升温:初始温度50℃(2 min),以5℃·min^-1速率升温到160℃,然后以4℃·min^-1速率升温至200℃,再以6℃·min^-1速率升温至250℃(10 min)。选择EI离子源,溶剂延迟2 min,质量扫描范围m/z 35~650。 结果: 生品白术和炒白术挥发油平均含量(n=3)分别为1.31%和0.98%;分别检出115和114个色谱峰,鉴定了其中58和60个化合物,占相应挥发油总量的93.84%和86.01%。其中,绝大多数为单萜或倍半萜类成分,主要成分包括:苍术酮(生白术中46.05%,炒白术中36.17%;下同)、γ-马榄烯(19.25%,16.78%)、6-异丙烯基-4,8a-二甲基-1,2,3,5,6,7,8,8a-八氢萘-2-酮(4.20%,3.04%)、β-桉叶烯(3.81%,4.13%)、3,7(11)-芹子二烯(3.36%,4.53%)、4,5-去氢异长叶烯(1.94%,1.85%)、去氢香橙烯(1.61%,2.30%)、γ-榄香烯(1.68%,0.95%)、去氢环异长叶烯(1.17%,1.19%)、石竹烯(1.12%,1.09%)、杜松脑(0.66%,1.08%)、白术内酯Ⅰ(1.27%,1.77%)、白术内酯Ⅱ(0.92%,1.51%)、白术内酯Ⅲ(0.44%,1.14%)和表白术内酯Ⅱ(0.31%,0.57%)等。 结论: 白术经炒制后挥发油总含量明显降低;生品白术和炒白术挥发油化学成分基本一致,但各主要成分含量存在明显差异。

Objective: To investigate the chemical components of essential oil from the rhizomes of Atractylodes macrocephala Koidz.(Atractylodis Macrocephalae Rhizoma; raw Baizhu; Sheng Baizhu) and its processed-product stir-fried with the bran(stir-fried Baizhu with the bran; Chao Baizhu), and study the chemical diversity after processing. Method: The classic water-steam distillation was adopted to obtain the essential oil and also calculate the oil yields, and GC-MS analysis was deployed to give out their chemical composition. A DB-5MS capillary column(30 m×0.25 mm×0.25 μm) was adopted with the vaporization temperature of 270℃. Heating program:the initial temperature was 50℃, kept for 2 min, then it was programmed to rise to 160℃ at a rate of 5℃·min^-1, followed with 4℃·min^-1 to 200℃, and then 6℃·min^-1 to 250℃, and then the temperature was maintained for 10 min. The electron impact(EI) ion source was selected and the solvent was delayed by 2 min, as well as the MS scanning was set at m/z 35-650. Results: The essential oil yield of Sheng Baizhu and Chao Baizhu accounted for 1.31% and 0.98% (n=3), respectively. One hundred and fifteen chromatographic peaks and one hundred and fourteen chromatographic peaks were detected from the Sheng Baizhu and Chao Baizhu essential oils, respectively. Among of them, 58 and 60 compounds were identified, which accounted for 93.84% and 86.01% of the total essential oil of Sheng Baizhu and Chao Baizhu, respectively. The overwhelming majority of the identified structures were monoterpenes and sesquiterpenes. The main components detected in the essential oil were atractylon (46.05% in Sheng Baizhu and 36.17% in Chao Baizhu; same order below), γ-maaliene (19.25% and 16.78%), 6-isopropenyl-4,8a-dimethyl-1,2,3,5,6,7,8,8a-octahydro-naphthalen-2-none (4.20% and 3.04%), β-eudesmene (3.81% and 4.13%), selina-3,7(11)-diene (3.36% and 4.53%), 4,5-dehydroisolongifolene (1.94% and 1.85%), dehydroaromadendrene (1.61% and 2.30%), γ-elemene (1.68% and 0.95%), dehydrocycloisolongifolene (1.17% and 1.19%), caryophyllene (1.12% and 1.09%), juniper camphor (0.66% and 1.08%), atractylenolide Ⅰ(1.27% and 1.77%), atractylenolide Ⅱ(0.92% and 1.51%), atractylenolide Ⅲ(0.44% and 1.14%) and epiatractylenolide Ⅱ(0.31% and 0.57%), etc. Conclusion: After frying process, there is a significant reduction of the essential oil yield of Rhizoma Atractylodis Macrocephalae. The components of essential oil of Rhizoma Atractylodis Macrocephalae before and after processing are basically the same, but there are significant differences of the contents.