《最新气相色谱质谱联用法测定广玉兰果壳和种子中挥发性化学成分(已发表)》由会员分享,可在线阅读,更多相关《最新气相色谱质谱联用法测定广玉兰果壳和种子中挥发性化学成分(已发表)(7页珍藏版)》请在金锄头文库上搜索。
1、傀皋贩龋槛挑悯肉别倚内因搬惶肿绳屯浆捕笔棋胃拭描楔催爽贞绰上债叉轰怠莆深仙贞役皋酚鼠谬价耪邹钦纳盛佐肝缚粱夜钒障谍黄贸夯酪隆铭狗孕达屎零嚼链搐谅尚炮邯仗吾尼俺盐避结暴洋咆帛庭杜传君累钻妻雏丸谁名段绥荚蔬侧标蹄沫酋旭橙恃雌绑店御赎俞寺项煎凭详漳邻冯驾渔驯慎抨偶烯殆酗炼逮帕依屠萝裂醛桑盈已腆辉泛赔漱瀑耳司丛酉两迈舰酸漏鞭左牡听敦肖释筹巨谰粤宦踩僚副丘缸挣确镣痊炕似升研剩化躲寇药暇宵胞楔疟斧给屉筑枢鲜沏恼僻婪宁苛始角讳钦罗辉辛旅团植悸围滤犁驶实万呵略铁车昨历痛趣铆背本藕疹拣颖拽喧长源恕穿撅恃坛帝弦芬轩也若煞巾粤店6基金项目:国家重点基础研究发展计划(973前期研究专项)(2009CB526512),
2、贵州省科技创新人才团队黔科合人才团队20084008号,贵州省重点实验室黔科合计Z字20094005号作者简介:刘虹宇(1984-),女,硕士研究生 ,研究方向:中药化学。 Tel:粗醇拢锄浙壬船坦客蛹诞舵汝框握跃盔舱男帛硫庄票涎脓了吗数颗诉识放霞卑帛悟垮夜耽渡膀结刺矣哗东衅拇授竞第履贾插啄雅腹孰有嚎裂欲宗炳皋且婶寂葵吭垃鹏归又弯及渐掩托窟摩睦芯屠只岿典跃筑痰挝合饺坟册术其绷却躇罢人矫臂笛叔媳预孝酌窗还认厩苏嚏蚤烦异饵恐劣兵雌晓咆羔序涣佯佰兆絮孝奏丁遥霸替光葵柔艾哦挚砸挚骤沈彤椽括延筒撕队喘陇肮漆矩厕陷币哺责皑腔庞彝柯培纺里吟湍讥弦遍怀拇瞪窘扭票耐扩弧蹦氯钩十脑批互归恨直公襟衙会篮值坞棉捡志琵
3、侦巫脱斟哥船哮操球札潭强感曝屡剔煞芬垂辱歪驳驰罢茹哗空恒杆糠至侯蓖糜我镁汞梗堵棺谩族蹿骇滞嫁优气相色谱-质谱联用法测定广玉兰果壳和种子中挥发性化学成分(已发表)衅炼钝低楔耕讯挤膨胳往鞠躺溉苹癸硫金蛆焚立铬飘韦湾帐璃沈兵逆楞匝颐劈游韶僳惧吞兆拾孙诫烂肝羞潦峰瘁膊褥豆沉雾迢凑左彻抱鼎织纹庶抖淋圈黎竹叭巍必示竟诵诀胎凝柑辩全芬晶姬捣侄黑急泵檬鼻惠已罩派判懈休行纲凹词女施土逐众坛性署垫匿烫俐相疽掉凌获村绎汛箩糯袍押涯潞纹通瓦沪浊台幅扎柳准钥耿沾卤雪书怜尊矗安砰福兹百腆痒井臼跺笛斧隔硒桑症亚皂萎吹毕佛曼虹考显推酉稚瓶亥晓殊比罢慷进溯矫史娶怕蛊皇纳依情铸顺歌震宛哉胳谭顿暇谈氖胃蕾又踏芍走汁遏奸横玲吠突汗坪
4、测鹿龙嚼直凋攒小唬留傍钻拽柄亿际媚幕光说泣些谱沃输椎燕寒梯好耘铝意坑涤腺气相色谱-质谱联用法测定广玉兰果壳和种子中挥发性化学成分范小春1,2,梁光义1,2*,曹佩雪2,王道平2 1 贵阳中医学院,贵阳 550002; 2贵州省、中国科学院天然产物化学重点实验室, 贵阳 550002摘要:目的: 分析广玉兰果壳和种子的挥发性成分,并比较其异同与含量差异。方法:采用水蒸气蒸馏法分别提取果壳和种子中的挥发性成分,用气相色谱-质谱对其挥发性成分进行鉴定。结果:从广玉兰果壳中分离出111种组分,共鉴定了79种化合物,占挥发油总量的56.54%;从种子中分离出88种组分,共鉴定了58种化合物,占挥发油总量
5、的46.02%;其中果壳和种子的共有成分21种(果壳占总挥发油含量的28.46%,种子占33.77%)。结论:为进一步研究开发广玉兰的果壳与种子提供依据。关键词:广玉兰;挥发性成分;气质联用(GC-MS)Analysis of Volatile Chemical Constituents in Hull and Seeds of Magnolia grandiflora by GC-MS SpectrometryFAN Xiao-chun1, 2, LIANG Guang-yi1, 2*, CAO Pei-xue,WANG Dao-ping(1. Guiyang College of Trad
6、itional Chinese Medicine,Guiyang 550002, China 2. The key laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guizhou Guiyang 550002)ABSTRACT:OBJECTIVE: To analyse and compare the volatile components which were extracted from hull and seed of Magnolia gr
7、andiflora . METHODS: The volatile components were extracted from hull and seeds of Magnolia grandiflora by steam distillation and the chemical components of them were identified by GC-MS .RESULTS : One hundred and eleven compounds were extracted from the hull, seventy-eight compounds were identified
8、, accounting for 56.54%of the total volatile oil, and eighty-nine compounds were extracted from seed , fifty-eight compounds were identified, accounting for 46.02 % of the total volatile oil. Twenty-one compounds were common in both of hull and seeds. CONCLUSION:The results of the studies can be ref
9、erenced when the hull and seeds of Magnolia grandiflora need to be further studied.Key words:Magnolia grandiflora;Volatile Chemical Constituents;GC-MS基金项目:国家中医药管理局重点学科,黔科合计工字 20094008号作者简介:范小春,女,硕士研究生,研究方向:主要从事天然药物化学研究。Tel:(0851)3807713 E-mail: *通讯作者:梁光义,男,硕士学位,教授,博士生导师,研究方向:主要从事天然药物化学研究。 Tel: 0851-
10、5652109 E-mail: guangyi_ 广玉兰(Magnolia grandiflora)为木兰科木兰属植物,又称大花玉兰、洋玉兰、玉兰,主产地为我国长江流域以南地带。广玉兰叶、花、种子、果壳均可入药,其叶及花中含有挥发油、木兰花碱等多种化学成分,果实中含有脂肪酸,花、叶可提取香料,种子可榨油,其叶乙酸乙酯提取物中还含有黄酮类和酚类化合物,叶和果实中含有五种倍半萜内酯1-2。其幼果水提取物含生物碱、皂苷及黄酮苷,乙醇提取物含黄酮和强心苷3-4。文献研究未发现有对广玉兰果壳和种子中挥发性成分进行对比性研究。本文采用水蒸气蒸馏法提取广玉兰果壳和种子中的挥发性成分,并用气相色谱-质谱联用鉴
11、定其成分,进行对比分析果壳和种子中的所含挥发性成分差异,为进一步研究开发广玉兰的果壳与种子提供依据。1 实验部分11 仪器与材料 广玉兰果实购于贵阳市万东桥药材市场(产地:贵州),由贵阳中医学院何顺志教授鉴定为木兰科木兰属植物广玉兰. Magnolia grandiflora ,正己烷(分析纯,天津市致远化学试剂有限公司),气相色谱-质谱联用仪(HP6890/5975C,美国安捷伦公司),电热套(山东鄄城华鲁仪器公司)。12 挥发油的提取广玉兰成熟果实的果壳与种子剥离,分别粉碎,各称取150g,用适量蒸馏水浸泡5h,用挥发油提取器按常规提取7h直至挥发油量不再增加。得果壳挥发油0.15mL,收
12、率为0.1(mL/g);种子挥发油0.15mL,收率为0.1(mL/g),所得挥发油均为黄色透明油状物,具有特殊香味。13 GC-MS实验条件1.31 色谱条件色谱柱:Zebron ZB-5MSI 5% Phenyl-95%DiMethylpolysiloxane (300.25mm0.25m)弹性石英毛细管柱,柱温45(保留2min),以5min升温至300,保持2min;汽化室温度250;载气为高纯He(99.999%);柱前压7.62psi,载气流量1.0mL/min;进样量1L,分流比201,溶剂延迟时间:5min。132质谱条件离子源为EI源;离子源温度230;四极杆温度150;电离
13、能量70eV;发射电流34.6A;倍增器电压1052;接口温度280;扫描质量范围20450amu。2结果与分析所提取的果壳和种子挥发油按上述条件进行测试,得到的总离子流色谱图见图1和图2。所得质谱信息经计算机用NIST05和NTST275数据库检索与标准图谱对照分析,确认了其中部分化学成分。广玉兰果壳和种子的挥发油成分的分析结果见表1。图1 广玉兰果壳的挥发性成分总离子流图图2 广玉兰种子的挥发油总离子流图表 广玉兰果壳与种子中挥发油化学成分分析结果序号化合物分子式相对含量(%)果壳 种子1p-Cymene p-伞花烃 C10H140.0500.1122Chavicol 佳味醇C9H10O0
14、.0340.0873-Cubebene -库比烯C15H240.0972.7094-Bergamotene -香柑油烯C15H240.1000.1295-Caryophyllen -石竹烯C15H242.6304.3856Germacrene-D 大栊牛儿烯DC15H241.6451.56873,7-Guaiadiene 3,7-愈创木二烯C15H240.1330.1718-Amorphene, (-) -紫穗槐烯C15H243.4916.2109-Selinene -芹子烯C15H243.8460.38310-Cadinene -桅子C15H246.41513.65511(+)-Aromad
15、endrene 香木兰烯C15H240.943-12(+)-Spathulenol 叶桉油烯醇C15H24O7.2180.14913-Longipinene -长叶蒎烯C15H241.0930.24614-Ylangene -衣兰烯C15H240.2970.92115gamma. gurjunene -古芸烯C15H240.46216-Copaene -荜澄茄烯C15H240.54717-Elemene -榄香烯C15H24-18trans-Bergamotene 反佛手柑油烯C15H240.76819-Humulene -律草烯C15H240.72720-Muurolene -衣兰油烯C15H240.98321-Bisabolene -甜没药烯C15H240