GCMS结合保留指数静态顶空进样分析木香挥发性成分

1、GC-MS结合保留指数静态顶空进样分析木香挥发性成分 山东省天然药物重点实验室大中药产业中药农业、中药商业、中药保健品、中药食品、中药兽药、中药美容、中药制药设备等-中药创新药物研究单元技术平台国家新药研发大平台（山东）4中药材饮片中药方剂数据库 中药及提取物样品库 中药复方中药创新组合药物中药创新组合药物产业化中药创新药物研究单元技术平台 饮片炮制子平台质量控制与评价子平台药理发现与评价研究子平台提取分离纯化子平台制剂研究子平台有效方剂临床发现子平台木香始载于神农本草经，为菊科植物木香Aucklandia lappa Decne.的干燥根。主产于云南，可行气止痛，健脾消食。临床上用于胸脘胀痛

2、，泻痢后重，食积不消，不思饮食。现代药理研究表明其挥发性成分对呼吸及心血管系统疾病有一定的对抗功效。本实验采用顶空进样技术，对木香挥发性成分进行了GC-MS分析，并结合保留指数（Kovats retention indices, KI）对其主要成分进行定性分析。仪器和试药GC 6890N气相色谱仪，MS 5975质谱仪，7694E顶空进样器正构烷烃混合对照品C8C40（美国AccuStandard公司，编号: DRH-008S-R2，500g/ml in Chloroform）木香Aucklandia lappa Decne.（产地：云南）挥发性成分的提取取新鲜粉碎的木香粉末（过40目筛）0.

3、5 g，准确称定，放入10 mL顶空瓶中密封，置顶空进样器中进样顶空条件：样品瓶加热温度120；样品环温度140；传输线温度160；样品瓶加热时间30 min，样品环平衡时间0.5 min，进样时间1 min。GC-MS分析条件色谱条件：色谱柱Agilent HP-5 MS (30m250m0.25m)；进样口温度250；载气为He气，柱流量1mL/min；程序升温条件：初始温度40，保持3min，以2/min升至150，保持2min，以10/min升到280。质谱条件：标准谱图调谐；电离方式EI，电子能量70 eV；离子源温度：230；数据采集扫描模式:全扫描，溶剂延迟时间：0.1min线性

4、升温公式计算各组分的KI值对木香顶空直接进样挥发性成分进行GC-MS分析。各峰质谱图进行NIST标准谱库检索，选取质谱匹配度高的前5个可能物质，计算其KI值，并与NIST库KI值检索结果相比较，以质谱和KI值匹配度最高的化学结构为最佳鉴定结果No.化合物KI*KI*分子式相对含量（%）1Hexanal800800 C6H12O0.25 2Furfural827829 C5H4O20.46 3Butanoic acid, 3-methyl-845851 C5H10O20.23 4Bicyclo3.1.0hex-2-ene, 2-methyl-5-(1-methylethyl)-925923 C1

5、0H160.54 5.alpha.-Pinene931928 C10H160.94 6Bicyclo3.1.0hexane, 4-methylene-1-(1-methylethyl)-970968 C10H162.13 7.beta.-Pinene972969 C10H163.43 8Furan, 2-pentyl-992990 C9H14O0.29 9.alpha.-Phellandrene10001000 C10H165.07 101,3-Cyclohexadiene, 1-methyl-4-(1-methylethyl)-10141013 C10H160.52 11Benzene, 1

6、-methyl-2-(1-methylethyl)-10221021 C10H142.13 12D-Limonene10261024 C10H160.84 131,3,6-Octatriene, 3,7-dimethyl-, (E)-10451038 C10H160.10 141,4-Cyclohexadiene, 1-methyl-4-(1-methylethyl)-10581055 C10H160.91 15Cyclohexene, 1-methyl-4-(1-methylethylidene)-10841084 C10H160.45 表1 木香挥发性化学成分GC-MS分析结果No.化合物

7、KI*KI*分子式相对含量（%）163-Cyclohexen-1-ol, 4-methyl-1-(1-methylethyl)-11741173 C10H18O0.35 172H-1-Benzopyran, 3,4,4a,5,6,8a-hexahydro-2,5,5,8a-tetramethyl-(2,4a,8a)-12891282 C13H22O0.12 18Cyclohexane,1-ethenyl-1-methyl-2,4-bis(1-methylethenyl)-,1S-(1.alpha.,2.beta.,4.beta.)-13911388 C15H2411.24 191H-Cyclo

8、propeazulene,decahydro-1,1,7-trimethyl-4-methylene-, 1aR-(1a,4a,7,7a,7b)-14011403 C15H240.52 20Caryophyllene14121412 C15H248.69 211H-Cyclopropaanaphthalene,1a,2,3,5,6,7,7a,7b-octahydro-1,1,7,7a-tetramethyl-, 1aR-(1a.alpha.,7.alpha.,7a.alpha.,7b.alpha.)-14321424 C15H242.58 22Bicyclo3.1.1hept-2-ene, 2

9、,6-dimethyl-6-(4-methyl-3-pentenyl)-14281432 C15H241.60 23Aromadendrene14391438 C15H240.08 24.alpha.-Caryophyllene14471446 C15H240.64 255,9-Undecadien-2-one, 6,10-dimethyl-14541452 C13H22O0.47 261H-Cyclopropeazulene, decahydro-1,1,7-trimethyl-4-methylene-, 1aR-(1a.alpha.,4a.beta.,7.alpha.,7a.beta.,7

10、b.alpha.)-14611456 C15H240.38 272-Isopropenyl-4a,8-dimethyl-1,2,3,4,4a,5,6,8a-octahydronaphthalene14741470 C15H240.37 28Spiro4.5dec-7-ene,1,8-dimethyl-4-(1-methylethenyl)-,1S-(1,4,5)-14831476 C15H242.53 293-Buten-2-one, 4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-14891483 C13H20O0.29 30Naphthalene,decahyd

11、ro-4a-methyl-1-methylene-7-(1-methylethenyl)-, 4aR-(4a,7,8a)-14861488 C15H240.97 No.化合物KI*KI*分子式相对含量（%）311-Pentadecene14941492 C15H302.43 32Azulene, 1,2,3,5,6,7,8,8a-octahydro-1,4-dimethyl-7-(1-methylethenyl)-, 1S-(1,7,8a)-15061498 C15H240.92 33Spiro2.5octane, 5,5-dimethyl-4-(3-oxobutyl)-15041506 C1

12、4H24O0.45 34-Farnesene15091512 C15H240.64 35Cyclohexene, 3-(1,5-dimethyl-4-hexenyl)-6-methylene-, S-(R*,S*)-15351521 C15H240.16 36Cyclohexanemethanol, 4-ethenyl-,4-trimethyl-3-(1-methylethenyl)-, 1R-(1,3,4)-15491545 C15H26O0.21 37Caryophyllene oxide15761575 C15H24O0.60 384-Hexadecen-6-yne, (Z)-16371655 C16H280.58 39Cedren-13-ol, 8-16881657 C15H24O0.92 409,12-Octadecadien-1-ol, (Z,E)-16721660 C14H26O2.52 414-Hexadecen-6-yne, (Z)-