温郁金中倍半萜类成分的分离与鉴定

目的对温郁金(Curcuma wenyujin)的化学成分进行研究。方法采用硅胶柱色谱、ODS柱色谱、Sephadex LH-20柱色谱,HPLC以及制备薄层色谱(P-TLC)进行分离和纯化,并依据理化性质和光谱学分析鉴定其化学结构。结果从温郁金的体积分数为50%的乙醇溶液提取物中分离得到6个倍半萜,分别鉴定为原莪术醇(procurcumenol,1)、环氧泽泻烯(alismoxide,2)、aeruginolac-tone(3)、(1E,4Z)-8-hydroxy-6-oxogermacra-1(10),4,7(11)-trieno-12,8-lactone(4)、1β,4α-di-hydroxy-5α,8β(H)-eudesm-7(11Z)-en-12,8-olide(5)和curcolonol(6)。结论其中化合物1、2为愈创木烷型倍半萜,3、4为吉玛烷型倍半萜,5、6为桉烷型倍半萜。化合物4、5均为首次从该属植物中分离得到,化合物1、2、3、6均为首次从本植物中分离得到。     

温莪术中的愈创木烷型倍半萜

目的对温莪术(Curcuma wenyujin)的化学成分进行研究。方法采用硅胶柱色谱、ODS柱色谱、Sephadex LH-20柱色谱以及HPLC进行分离和纯化,并依据理化性质和谱学分析鉴定其化学结构。结果从温莪术的体积分数为50%的乙醇溶液提取物中分离得到7个愈创木烷型倍半萜,分别鉴定为zedoarondiol(1)i、sozedoarondiol(2)a、erugidiol(3)z、edoalactone A(4)z、edoalactone B(5)、zedoalactone C(6)和zedoarolide B(7)。结论化合物1-7均为首次从该植物中分离得到。     

不同产地莪术挥发油的研究

目的：研究不同产地莪术挥发油的化学成分，了解同产地莪术挥发性成分的差别，为控制莪术挥发油的质量提供理论依据。方法：采用水蒸气蒸馏法提取不同产地莪术挥发油，用气相色谱－质谱联用仪对其进行分离测定，结合计算机检索对分离的化合物进行结构鉴定。应用色谱峰面积归一化法测定各成分的相对百分含量，结果：不同产地莪术水蒸气蒸馏提取物得率在在0．26％－0．35％之间，分别鉴定出29－42个化学成份。结论：不同品种，不同产地莪术挥发性成分有较大差别，主要为萜类及倍半萜衍生物。     

温郁金中的新桉叶烷型倍半萜內酯

为了研究温郁金(Curcuma wenyujin Y.H. Chen et C. Ling)根茎中的倍半萜类成分，采用大孔树脂和反复硅胶柱色谱对温郁金干燥根茎的50%乙醇提取物进行分离纯化，得到8个倍半萜类化合物1～8；其化学结构通过多种波谱方法分别鉴定为温郁金内酯A(wenyujinlactone A，1)、neolitamone A (2)、zedoarondiol (3)、isozedoarondiol (4)、aerugidiol (5)、莪术醇(curcumol，6)、莪二酮(curdione，7)和(1R,10R)-epoxy-(-)-1,10-dihydrocurdine (8)。化合物1为新的桉叶烷型倍半萜内酯，化合物2～5为首次从该植物中分离得到。     

Analysis of volatile components of Curcuma sichuanensis X. X. Chen by gas chromatography-mass spectrometry

Volatile components of Curcuma sichuanensis X. X. Chen growing in Sichuan, China, were extracted by steam distillation and analyzed by using gas chromatography and gas chromatography-mass spectrometry. A total of 44 volatile essential oil components were identified in the extract of C. sichuanensis X. X. Chen, representing 87.1% of the total integrated chromatographic peaks. The major compounds were found to be epi-curzerenone (26.9%), germacrone (12.4%), isocurcumenol (9.7%), beta-elemene (6.4%) and curzerene (6.2%). The results of semi-quantitative analysis indicated that levels of total sesquiterpene fraction (85.4%) were more than 55 times higher than those of monoterpene components (1.5%).     

伊痛舒注射液中挥发油的GC-MS分析

目的对伊痛舒注射液中挥发油成分进行GC-MS分析。方法利用水蒸气蒸馏法提取伊痛舒注射液全方以及单味药材中的挥发油成分,利用GC-MS联用技术,结合计算机Nist-base质谱库检索技术,根据匹配度,对分离的化合物进行初步鉴别,分析伊痛舒注射液全方中挥发油成分的来源。结果伊痛舒注射液全方经水蒸气蒸馏提取,GC-MS分析,共得到59个色谱峰,鉴定了其中39个成分,占挥发性物质含量的53.27%。结论根据保留时间以及计算机质谱库对每个化合物给出的鉴定,分析了这39个成分的来源,其中防风、川芎和羌活对这39个成分的出现起了主要的作用,其次为其他。     

刺五加叶挥发性化学成分的提取与气相色谱-质谱分析

目的:比较不同提取方法对刺五加叶中挥发性化学成分的得率,并对其挥发性化学成分进行分析。方法:采用同时蒸馏萃取法(SDE)与常规提取法(水蒸气蒸馏法、溶剂法)对刺五加叶药材挥发性化学成分的提取收率进行比较研究,用GC/MS法对其挥发性化学成分进行分离鉴定,用峰面积归一化法得出各化学成分在挥发性组分中的相对百分含量。结果:共分离出51个成分,确认了其中39种化学成分,主要为萜类及其含氧衍生物(68.85%)和芳香族类化合物(6.32%),其中,(+)匙-叶桉油烯醇含量最高,达19.89%,其余依次为1甲-基-5亚-甲基-8-[1甲-基乙基]-1,6环-癸二烯(7.02%)和1甲-基-1乙-烯基-2,4二-异丙烯基-环己烷(5.59%)等。结论:同时蒸馏萃取法是提取刺五加叶挥发性物质的优良方法。采用GC-MS法可以高效、适用、准确地分析、鉴定药材中挥发性物质的组成,对深入探索中药的药用价值具有积极的促进作用。     

温郁金的化学成分和药理作用研究进展

温郁金为浙江省道地传统中药材,应用广泛,所含化学成分种类繁多,主要有挥发油、姜黄素类、生物碱等。药理学研究表明,温郁金具有抗肿瘤、抗炎镇痛、抗病毒、保护心血管系统、保护神经、抗氧化、保肝、细胞毒等作用。总结温郁金的主要化学成分和药理学作用的研究进展,以期为温郁金的进一步开发研究和合理用药提供参考。     

Headspace solvent microextraction-gas chromatography-mass spectrometry for the analysis of volatile compounds from Foeniculum vulgare Mill

A novel and rapid headspace solvent microextraction followed by gas chromatography-mass spectrometry (HSME-GC-MS) for the analysis of the volatile compounds of Foeniculum vulgare Mill is described. HSME parameters including extracting solvent, extraction temperature and time, headspace volume and particle size were optimized. As a result, benzyl alcohol was finally used for the extraction at 70 degrees C for 20 min with headspace volume of 12.1 ml and particle size of 120 mesh. Under the determined conditions, the powered samples of Foeniculum vulgare Mill were directly applied for the analysis. A comparison of HSME-GC-MS, solid phase microextraction (SPME)-GC-MS and steam distillation (SD)-GC-MS methods was made and showed that the HSME-GC-MS method was simple, inexpensive and effective and can be used for the analysis of volatile compounds in traditional Chinese medicines (TCMs).     

板栗花的挥发油成分

板栗花的挥发油经 PEG—20M 玻璃毛细管柱分离出52个组分,用 GC—MS 分析法鉴定了33个化合物。抑菌实验表明该挥发油具有抗菌作用。     

固相微萃取/气-质联用法分析香连制剂中挥发性成分

目的： 利用固相微萃取/气相色谱-质谱联用法（SPME/GC-MS）分析香连制剂（水丸/浓缩丸/片/胶囊）中的挥发性成分。方法： 采用SPME法提取挥发性成分,GC-MS法对挥发性成分进行分离鉴定,建立其指纹图谱,并对香连制剂样品进行相似度评价和主成分分析。结果： 对24批不同剂型香连制剂进行分析,确定了15个共有峰,构成了香连制剂挥发性成分的指纹图谱,其中6个共有峰得到了确认,分别为去氢木香内酯,β-榄香烯,β-石竹烯,氧化石竹烯,α-紫罗兰酮和β-紫罗兰酮。结论： 水丸、浓缩丸与片剂、胶囊中挥发性成分组成相似,但在相对含量上存在差异。     

Study of components in crude drugs by head space gas chromatography. I. Components of Asiasari radix

Determinations of volatile components of essential oil contained in Asiasari Radix were studied by head space gas chromatography. The head space gas, which was generated by heating 0.2 g of crude drug with 1.0 ml of water at 90 degrees C for 45 min, was analyzed directly by gas chromatography or gas chromatography-mass spectrometry. This method was rapid, and did not require tedious procedures and time consuming, and without contamination of the column.     

广西莪术的叶、根茎和块根中挥发油GC-MS对比分析

目的：对广西莪术叶中挥发油成分进行系统的分析,并与其传统的用药部位块根和根茎的挥发油成分对比,寻找广西莪术叶作为代替性药材的可能性,尽可能的扩大广西莪术的药用部位,提高广西莪术整株植物的经济效益。方法：采用水蒸气蒸馏法提取挥发油,运用GC/MS方法比较叶与根茎,块根的化学成分及其各成分的相对百分含量。结果：从广西莪术叶中分离得到38个色谱峰,鉴定出26种成分。结论：首次从广西莪术叶中鉴定出26种挥发性成分,叶中所含成分与根茎、块根的差别较大,但也含有部分抗肿瘤成分。     

Phytochemical and Antiplatelet Investigation of Gundelia tournifortii.

ABSTRACT

Five known compounds from the aerial parts of Gundelia tournifortii. L. (scopoletin, isoscopoletin, esculin, and a mixture of β.-sitosterol and stigmasterol) were isolated and identified on the basis of spectral evidence (¹H NMR, ¹³C NMR, MS, and IR). The volatile oil from aerial parts of G. tournifortii. was obtained by hydrodistillation, for the first time, and its composition was determined by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). alpha-Terpinyl acetate (36.21%), methyl eugenol (12.57%), eugenol (6.7%), β.-caryophellene (5.94%), and zingiberene (5.84%) were the major oil components. The antiplatelet activity of G. tournifortii. was studied in vitro. using adenosine-5′-diphosphate (ADP) and arachidonic acid (AA) as agonists. The chloroform extract of G. tournifortii. was found to have a mild inhibitory effect on platelet aggregation induced by ADP and AA. None of the pure isolated compounds or the volatile oil showed an inhibitory effect on platelet aggregation using ADP and AA as agonists.     

GC-MS结合保留指数分析侧柏叶挥发成分

目的分析比较不同采集方法制备的侧柏叶中的挥发性成分。方法分别采用水蒸气蒸馏法和顶空加热提取挥发性成分的方法,对其进行气相色谱-质谱（GC-MS）分析,并结合Kovats保留指数对其主要成分进行定性分析。结果采用顶空进样技术,可鉴定出侧柏叶中29个挥发性化学成分;采用水蒸气蒸馏法可鉴定出34个挥发性化学成分;两种采样方法进行的GC-MS分析,有23种相同化合物,但相对含量有一定差异。结论对于侧柏叶,水蒸气蒸馏法提取挥发性成分较完全,顶空直接进样对于易挥发性成分分析则更简便、高效。     

气相色谱-质谱联用技术分析蕲艾籽中挥发性成分

目的：用气相色谱-质谱联用技术分析蕲艾籽中挥发性成分。方法：分别采用水蒸气蒸馏法（SD）和顶空-固相微萃取法（HS-SPME）提取蕲艾籽挥发性成分,通过气质联用（GC-MS）技术分析其化学成分组成,并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：采用SD-GC-MS法共分离出33个色谱峰,鉴定出其中29个化合物,占总挥发性成分的93.02%;采用HS-SPME-GC-MS法共分离出35个色谱峰,鉴定出其中30个化合物,占总挥发性成分的99.01%。通过这两种技术共同鉴定出的挥发性成分共有11种,其中含量最高的成分为β-侧柏酮。结论：SD与HS-SPME鉴定出的挥发性成分及其相对含量上存在一定差异,两者适用于不同类型的挥发性成分的提取,将两者联用分析蕲艾籽挥发性成分能够得到更加全面的信息。     

Quinoline alkaloids,coumarins and volatile constituents of Helietta longifoliata

A new quinoline alkaloid named helietidine ( 1), and seven known compounds ( 2 - 8) have been isolated from the stem barks of Helietta longifoliata. The structures of the new and the known compounds were established on the basis of spectral evidence, especially by 2D NMR ( 1H- 1H COSY, NOESY, HMQC, HMBC). In addition, the volatile constituents of H. longifoliata leaves were analysed by gas chromatography-mass spectrometry (GC-MS). Twenty-five constituents were identified representing ca. of 96 % of the oil, and limonene (17.50 %), germacrene D (16.60 %), elemol (11.81 %), bicyclogermacrene (11.67 %), guaiol (11.53), and epi-alpha-bisabolol (7.24 %) were the most abundant components. The oil was bioactive against some Gram-positive and Gram-negative bacteria, as revealed by bioautography.     

黑老虎药材挥发油成分超临界CO_2萃取与水蒸汽蒸馏工艺比较

目的研究黑老虎药材用2种不同提取方法所得挥发油成分及收率。方法用超临界CO2萃取技术及水蒸汽蒸馏法从黑老虎药材中分离出挥发油,并用气相色谱/质谱联用技术测定其化学成分。结果从2种不同方法所得挥发油中分别鉴定出27种和25种成分。其中β-石竹烯、δ-杜松烯、法尼醇、芹子烯为黑老虎药材挥发油的主要成分。结论超临界CO2萃取法比水蒸汽蒸馏法从黑老虎中分离的挥发油收率高,且工艺耗时少。     

柠檬桉叶挥发油化学成分气相色谱-质谱分析研究

目的 研究广东产柠檬桉叶挥发油的化学成分.方法 采用水蒸气蒸馏法提取广东产柠檬桉叶挥发油,用气相色谱-质谱联用技术进行分离测定,结合计算机检索技术对分离的化合物进行结构鉴定,应用气相色谱峰面积归一化法确定各组成分的相对含量.结果 首次确定了广东产柠檬桉叶挥发油中33个化合物,其主要成分是薄荷醇(34.33％)、新薄荷醇(16.11％)、右旋香茅醇(13.93％)、香茅醛(12.42％)、孟二醇(5.16％)等.采用峰面积归一法计算各组分的相对含量,所鉴定成分占总馏出峰面积的96.07％.结论 确定了广东产柠檬桉叶挥发油的化学成分,与文献报道具有相似性,但仍存在差别,结果提示下一步有必要对柠檬桉叶挥发油成分新的药理作用进行深入研究,为综合利用柠檬桉叶挥发油奠定基础.