超临界CO2萃取冬虫夏草子座挥发性成分的GC-MS研究

报道冬虫夏草挥发性成分的组成,为其进一步的研究工作奠定基础。采用超临界CO2萃取法从冬虫夏草子座中提取挥发性成分,气相色谱-质谱联用技术对其化学成分进行分析。超临界流体萃取物共鉴定了39种组分,占总馏出组分的86.6%以上,占色谱总馏出峰面积的98.56%以上。已鉴定组分中,含量最高的为油酸,相对含量25.6%;其次为亚油酸,相对含量22.67%;再次为棕榈酸11.86%。超临界CO2萃取法能更真实、全面的反映药材中的化学成分,适合于珍稀中药材相关组分的测定。     

不同提取方法对印度紫檀叶片挥发性成分的GC-MS分析

采用气相色谱-质谱法(GC-MS)分析同时蒸馏萃取法(SDE)、固相微萃取法(SPME)和动态顶空吸附法(DHA)三种方法提取的印度紫檀挥发性成分。结果表明:三种方法提取印度紫檀挥发油的化学成分有差异。同时蒸馏萃取法提取印度紫檀挥发油鉴定出25种化合物,主要成分为2-硝基乙醇,相对含量为35.29%;固相微萃取法提取印度紫檀挥发油鉴定出27种化合物,主要成分为乙酸叶醇酯,相对含量为33.62%;动态顶空吸附法提取印度紫檀挥发油鉴定出27种化合物,主要成分为2-硝基乙醇,相对含量为30.42%。三种方法共检测到2种相同组分,检出的主要物质是醇类、酯类和缩醛。     

基于GLME/GC-MS分析黄柄钙皮菌的挥发性成分

为分析黄柄钙皮菌的挥发性成分组成,通过气液微萃取技术(GLME)对无饲培养获得的黄柄钙皮菌中萃取挥发性成分,应用气相色谱-质谱(GC-MS)联用技术对其化学成分进行分析。共鉴定了66种组分,占总组分的56.41%以上,占色谱出峰面积的65.58%以上。已经鉴定的组分中,含量最高的是棕榈酸,相对含量是12.12%,其次是二十六烷。组分主要归为酸、酯、烷烃、醇、酮、醛等几大类化合物。研究结果表明GLME/GC-MS萃取技术较适用于黄柄钙皮菌等黏菌的挥发性成分的检测分析,为进一步研究黏菌的挥发性成分提供新的检测技术。     

基于不同提取方法的汉麻茎叶精油全组分鉴定及比较研究

以汉麻茎叶为原料,分别采用水蒸馏提取法、亚临界萃取法以及超临界萃取法来获得汉麻精油,比较不同提取方法下获得的精油全组分的差异性、特征性。采用气相色谱-质谱法(GC-MS)对精油全组分进行鉴定分析,并通过NIST质谱库和人工解析对所提取成分进行鉴别分析和相似度的检索,最后根据峰面积归一化法得出这三种提取方式下汉麻精油各组分的相对含量。三种提取方法下所得精油组分差异性明显,共计鉴定出154个成分,且含有13个共有成分,相似度均在80%以上。其中水蒸馏提取法共鉴定出89种,含量最高组分是大麻二酚(19.69%);亚临界萃取法鉴定出62种,含量最高组分是邻苯二甲酸二正辛酯(17.56%);超临界萃取法鉴定出59种,含量最高组分是油酸(22.50%)。三种方法所得精油组分种类和含量均有不同程度的差异：水蒸馏法获得的精油组分种类最多,多为烷烃、烯烃、醇类、醛类、倍半萜类等小分子化合物,而亚临界法和超临界法在一定程度上具有相似性,二者共有40个共有成分,多为酸类,醇类,酯类,酚类等高沸点化合物或大分子化合物,但含量差异明显。     

兴安杜鹃叶中挥发性成分的GC-MS分析

采用水蒸气蒸馏法对兴安杜鹃叶中的挥发性成分进行提取,并运用气相色谱—质谱联用技术(GC-MS)对其挥发性成分进行了系统的分离和鉴定。从兴安杜鹃叶中共鉴定出54种挥发性成分,占总馏出成分的97.84%。兴安杜鹃叶主要挥发性成分为桉叶醇(eduesmol),相对含量10.95%;β-愈创木烯(β-guaiene),相对含量10.21%;长叶醛(longifolenaldehyde),相对含量7.88%;1,5,9,9-四甲基-1,4,7-环十一碳三烯(1,5,9,9-tetramethyl-1,4,7-cy-cloundecatriene),相对含量7.80%;杜鹃酮(germacrone),相对含量5.91%;(-)-葎草烯环氧化物Ⅱ((-)-HumuleneepoxideⅡ),相对含量5.52%;2-庚基-1,3-二氧戊环(2-heptyl-1,3-dioxolane),相对含量4.99%;石竹烯(caryo-phyllene),相对含量3.70%;(+)-γ-古芸烯((+)-γ-gurjunene),相对含量3.44%。     

石油菜挥发油和超临界流体萃取物化学成分的GC-MS分析

首次利用水蒸气蒸馏法和超临界流体萃取法(SFE)对石油菜地上部位进行提取,分别获得挥发油和SFE萃取物,采用气相色谱-质谱联用技术(GC-MS)结合计算机数据库检索对这两种提取物的化学成分进行了分析鉴定,采用峰面积归一化法测定了其中各个化学成分的相对含量。从挥发油中共分离出39个色谱峰,鉴定了其中28个化学成分,已鉴定出的成分的相对含量总和占化合物检出总量的91.90%,化合物类型均为萜类。从SFE萃取物中共分离出136个色谱峰,鉴定了其中65个化学成分,已鉴定出的成分的相对含量总和占化合物检出总量的58.17%,化合物类型包括萜类、芳香族类和脂肪族类。挥发油和SFE萃取物均含有α-蒎烯、石竹烯和桉油烯醇,其他成分则存在较大差异。     

超临界柚子鲜花芳香性成分的研究

本文介绍了采用超临界CO2萃取新鲜柚子花中芳香性成分,并用气相色谱-质谱联用仪对其中化学成分进行分析鉴定.共鉴定出31个芳香性有机化学成分,占超临界CO2萃取柚子鲜花总芳香油的78.886%.通过对柚子花芳香性成分的分析,为开发高附加值的柚子花香精香料提供科学依据.     

桑寄生挥发性成分研究

目的：研究桑寄生（Herba Taxilli）中的挥发性成分。方法：利用水蒸气蒸馏法提取桑寄生挥发油,用GC/MS进行测定,结合计算机检索技术对分离的化合物进行结构鉴定,应用色谱峰面积归一化法计算各成分的相对百分含量。结果：分离出132个组分,鉴定出66个化学成分。检出率为78.91%。桑寄生挥发性成分大于2%的为苯甲醛13.97%,苯乙烯11.42%,芳姜黄烯7.89%,桉树脑3.89%,α-姜烯3.59%,γ-姜黄烯2.78%,壬醛2.07%。     

超临界CO2萃取茉莉净油化学成分的研究

利用 GC和 GC- MS联用仪对超临界 CO2 萃取茉莉浸膏的净油进行化学成分分析 ,分离出 131个组分 ,鉴定出其中的 35个化合物 ,所鉴定的成分占分离成分的 85%以上。同时将分析结果与普通溶剂法制取的茉莉净油进行比较。     

白果油的提取工艺及其化学成分研究

采用正交实验对超临界CO2萃取白果油的工艺条件进行优化,比较超声波提取、索氏提取、超临界CO2萃取3种方式对白果油提取率的大小,用最佳提取方式分析不同品种白果中油脂的含量,并用GC-MS分析其成分.结果表明: (1)3种提取方式对白果油提取率的大小顺序为:超临界CO2萃取(添加夹带剂)＞索氏提取＞超声波提取.(2)超临界CO2萃取白果油的最佳工艺条件为:温度40℃、压力20 MPa、流速15 L/h、时间3 h并添加石油醚夹带剂,不同品种白果干粉中油脂得率为3.6%～7.11%.(3)GC-MS分析表明:从超临界萃取白果油中鉴定出17种化学成分,其中不饱和脂肪酸占85.4%;超声波和索氏提取相似,分别从提取的白果油中鉴定出10种和9种化学成分,其中不饱和脂肪酸含量分别为90.3%和90.1%;不饱和脂肪酸以十六、十八碳的为主.     

花椒挥发油的超临界CO2萃取法与水蒸气蒸馏法提取的比较

采用超临界萃取法与水蒸气蒸馏法从花椒中提取花椒挥发油,用GC—MS方法测定各种提取方法得到挥发油的化学成分及相对含量。结果表明,水蒸气提取挥发得率为3．8％（W／W）,主要成分为柠檬烯（22．75％）、沉香醇（21．70％）、罗勒烯（3,7-二甲基-1,3,7-辛三烯）（14．27％）等。超临界CO2萃取法挥发油得率为5．9％（W／W）,主要成分为柠檬烯（14．01％）、沉香醇（13．18％）、罗勒烯（3,7-二甲基-1,3,7-辛三烯）（26．23％）等。两种方法所得到的挥发进行比较,水蒸气蒸馏法分离法得到的挥发油中分离出78个峰,其中含量和相似度高的成分有31种,占86．31％。超临界CO2萃取法提取的花椒挥发油中分离出了152个峰,含量和相似度高的成分有36种,占74．72％。两种提取方法所得到的主要挥发油中有27种成分相同。     

人工培养蛹虫草与野生冬虫夏草氨基酸含量的比较

对人工培养蛹虫草与青海产野生冬虫夏草的氨基酸含量进行测定,结果表明:野生冬虫夏草中所含有的各种氨基酸,在人工培养虫草的子实体及菌丝体中都有存在;且后者的精氨酸及脯氨酸含量明显高于野生冬虫夏草。由此为鉴定人工培养虫草的质量,进一步为工业规模开发与利用人工培养虫草,提供了科学理论依据。     

HPLC comparison of supercritical fluid extraction and solvent extraction of coumarins from the peel of Citrus maxima fruit

The efficiency of carbon dioxide supercritical fluid extraction (SFE) of the biologically active compounds imperatorin, meranzin and meranzin hydrate from the fruit peel of Citrus maxima Merr. has been compared with that of solvent extraction with acetone. Under the best SFE conditions tested for the three coumarins, which involved extraction at 50 degrees C and 27.6 MPa, the extractive efficiencies were 84, 76 and 18% for imperatorin, meranzin and meranzin hydrate, respectively. The presence of modifiers significantly affected the extraction efficiency: the highest extraction efficiency of the three coumarins was obtained with ethanol as modifier.     

北细辛超临界萃取物挥发性成分的GC-MS分析

采用超临界流体萃取法(SFE)和水蒸气蒸馏法分别对北细辛根及根茎进行提取分离,分别得5.5%SFE萃取物和2.8%挥发油。应用GC-MS分析,从北细辛SFE萃取物中鉴定出7种化学成分,占萃取物总量的72.70%,其中甲基丁香酚为44.62%;从细辛挥发油中鉴定出19种化学成分,占挥发油总量的88.53%,其中甲基丁香酚为43.02%。两种方法有6种成分完全相同,其中致癌物质黄樟油素SFE法比蒸馏法低2.8倍。北细辛根及根茎超临界萃取物与水蒸汽蒸馏挥发油主要成分相同,但其化学组成存在较大差异,提示药效亦不相同。超临界流体萃取法是剂型改革的有效方法之一。     

Supercritical-fluid extraction of synthetic pyrethroids from wool

A stepwise approach was used to develop a supercritical fluid extraction (SFE) method for analysis of synthetic pyrethroids (SPs) on a wool matrix, commencing with a simple inert matrix to examine the solubility of the pyrethroids in the extraction fluid CO(2) and then extended to the real wool matrix. Chemometric approaches were used to determine the SFE optimum conditions. It was found that pyrethroids were readily extractable from an inert matrix over a wide range of pressure (170-350 atm) and at low temperature (<90 degrees C). Subambient hexane efficiently trapped the compounds from the depressurised fluid. Excessively high pressure and temperature resulted in poor trapping, isomerisation and possibly degradation of some components. With spiked wool samples method modifications focused on reducing the coextraction of grease, a bulk matrix component of raw wool. By using alumina (containing 8% moisture) and operating the extraction at 50 degrees C, 200 atm for 60 min, sufficiently clean extracts of pyrethroids suitable for gas chromatography-electron-capture detection analysis were obtained. The recoveries of all SPs were satisfactory (78-101%) over the range of 0.5-5 microg/g levels of these compounds. The precision of the entire analysis procedure was comparable to the conventional Soxhlet extraction method. Detection limits of some commonly used SPs for sheep treatment were also evaluated. Comparable results relative to those achieved by solvent extraction for incurred wool samples were obtained with a recovery of 81-85%. The results, however, suffered high uncertainties (R.S.D. approximately 19-24%) due to the small amount of wool sample taken in each extraction and the suspected inhomogeneity of the wool. Different persistences of cypermethrin isomers in wool were observed.     

Identification of volatiles from differently aged red clover (Trifolium pratense) root extracts and behavioural responses of clover root borer (Hylastinus obscurus) (Marsham) (Coleoptera: Scolytidae) to them

Root extracts from 1.5 and 2.5-year-old red clover (Trifolium pratense) were obtained using supercritical fluid extraction (SFE). GC–MS analysis and Kovats indices allowed identification of the volatile compounds as butyl acetate, E-2-hexenal, α-pinene, benzaldehyde, 6-methyl-5-hepten-2-one, limonene, acetophenone, methyl benzoate, nonanal, octanoic acid and decanal.     

冬虫夏草及人工虫草菌丝体的氨基酸营养

本文研究了天然虫草菌与人工虫草菌的氨基酸含量。结果表明,天然虫草菌、人工虫草菌的总氨基酸含量稍有差异,但中性、酸性、碱性氨基酸和必需氨基酸在总氨基酸中所占百分比的高低基本一致。     

人工培殖冬虫夏草D-甘露醇的含量测定

采用水提回流离心的方法,提取分离人工培殖冬虫夏草中D-甘露醇,用高碘酸钠与甘露醇反应产生黄色的3,5-二乙酰-1,4-脱氢二甲基吡啶,在波长412 nm处测定其最大吸收.甘露醇浓度在10～50 mg/L之间时,与吸光值(OD412)有良好线性关系,线性方程为C=79.172x-0.0713,相关系数r=0.9999.人工培殖冬虫夏草中D-甘露醇的含量分别为89.64 mg/g(2005年)、91.86 mg/g(2006年)、94.71 mg/g(2007年)、98.98 mg/g(2008年)、97.50 mg/g(2009年)、94.71 mg/g(野生)和96.84 mg/g(野生).人工培殖冬虫夏草与野生冬虫夏草D-甘露醇的含量基本相同.     

Determination of the anamorph of Cordyceps sinensis inferred from the analysis of the ribosomal DNA internal transcribed spacers and 5.8S rDNA

The anamorph determination of Cordyceps sinensis remains problematic due to the lack of clear links between the sexual and conidial forms of the fungus. In this study, we applied molecular approaches to analyze the genetic variation of Cordyceps sinensis and its allies to identify the anamorph-teleomorph connection. The sequences of the internal transcribed spacers (ITS1 and ITS2) and 5.8S ribosomal RNA gene of Cordyceps sinensis (teleomorph) collected from Qingzang plateau (altitude over 4000m), Tibet and several related asexual conidial forms were determined. The sequence comparison showed that Cordyceps sinensis was most closely related to Hirsutella sinensis, and was clearly divergent from Paecilomyces sinensis, Stachybotrys sp. or Tolypocladium sp.; distance values, estimated according to Kimura two-parameter models between Cordyceps sinensis and Hirsutella sinensis, were extremely low (<0.02), whereas distance values between Cordyceps sinensis and Paecilomyces sinensis, Stachybotrys sp. and Tolypocladium sp. were 0.34, 0.21 and 0.25, respectively. Taken together, Hirsutella sinensis and Cordyceps sinensis are the different stages of the life cycle stages of the same organism. Hirsutella sinensis is therefore the anamorph of Cordyceps sinensis, rather than Paecilomyces sinensis or other species. The possible reasons as to why different taxa can be obtained when culturing Cordyceps sinensis are also discussed.     

虫草及其无性型中的抗肿瘤细胞活性成分

较系统地总结了目前在虫草及其无性型中发现的抗肿瘤细胞活性成分.其中冬虫夏草、蛹虫草、大团囊虫草、单侧虫草、戴氏虫草和拟蛹虫草等虫草以及它们的无性型蛹拟青霉、细脚拟青霉、金龟子绿僵菌和球孢白僵菌等虫生真菌代谢物中抗肿瘤细胞活性成分,其结构包括多糖类、甾醇类、含氮化合物和杂环化合物等多个类型.