沉香中精油的超临界CO_2萃取及其GC-MS分析

目的 用超临界CO2流体萃取沉香中的精油.方法 采用正交试验优化超临界CO2流体萃取沉香精油的工艺,并用GC-MS分析其化学成分.结果与结论 最佳工艺条件为:萃取压力18 Mpa、萃取温度40℃、萃取时间2 h、沉香药材粉末过40目筛,萃取率达0.62%;共分离出39个组分,鉴定了其中的34个成分.首次分离出γ-芹子烯、α-可巴烯-8-醇、广藿香醇(3种倍半萜化合物)、5-羟基-7-甲氧基-2-戊色酮、8-甲氧基-2-(2-苯乙基)色烯-4-酮、7-苄氧基-甲酰色烯-4酮(3种色酮化合物).     

超临界CO_2萃取与水蒸气蒸馏法提取太子参挥发油化学成分气质联用研究

目的:分析比较采用超临界CO2流体萃取法与水蒸气蒸馏法提取的太子参提取物中挥发性化学成分的异同。方法:使用水蒸馏提取法和超临界CO2萃取技术从太子参中提取挥发性成分,用归一化法测定其百分含量。用气相色谱-质谱(GC-MS)计算机联用技术分离鉴定其中的化学组成。结果:太子参超临界CO2流体萃取物中初步鉴定了33种成分,主要成分为:亚油酸乙酯(28.70%)、n-十六酸(23.12%)、3-糠醇(5.51%)等;水蒸气蒸馏法提取挥发油初步鉴定了17种成分,主要成分为2-丙基呋喃(22.45%)、3-糠醇(19.78%)、3-乙基-3-甲基戊烷(19.47%)。结论:2种方法提取的挥发油化学成分差异较大,超临界CO2流体萃取法提取的挥发油能更真实、全面地反映太子参药材中的化学成分。     

藏药甘毕二汤二氧化碳超临界流体萃取精油化学成分研究

目的:研究藏药甘毕二汤二氧化碳超临界流体萃取精油的化学组成及相对含量。方法:采用气相色谱-质谱联用方法分离鉴定甘毕二汤二氧化碳超临界流体萃取精油化学成分并测定其相对含量。结果:甘毕二汤二氧化碳超临界流体萃取精油得率为5.9%,分离得到48个色谱峰,鉴定出43种成分,主要成分是桉叶油二烯-5,11(13)-内酯-8,12、胡椒碱、β-谷甾醇、α-蛇麻烯、8-十七烯、9-十八炔酸甲酯、反亚油酸甲酯、榄香醇、正十六烷、花生四烯酸甲基酯、正十四烷、反式石竹烯、(Z,Z,Z)-9,12,15-十八烷三烯酸乙酯、1,1-二甲基萘等。结论:甘毕二汤二氧化碳超临界流体萃取精油中富含烃、萜、酯和醇等组分,其中桉叶油二烯-5,11(13)-内酯-8,12和胡椒碱的相对含量之和占精油含量的39.40%。     

金玄痔科熏洗散方中植物药超临界CO2萃取物的GC-MS分析

目的：分析金玄痔科熏洗散方中植物药超临界CO2萃取物的化学成分组成,诠释该中药复方制剂的药效物质基础。方法：采用超临界CO2萃取法得到超临界CO2萃取物,通过气相色谱-质谱法对其成分进行了分析鉴定。结果：共分离出34种成分,鉴定了其中33种化合物;主要成分为胡薄荷酮（23．17％）,棕榈酸（17．31％）、顺5-甲基-2-（1-甲基乙基）环己酮（11．74％）。结论：分析鉴定了金玄痔科熏洗散方中植物药超临界CO2萃取物有效物质部位中的33种化合物,占其总量的99％以上．这对于诠释该中药复方制剂的药效物质基础具有重要意义。     

广东海风藤超临界流体萃取物的气相色谱-质谱联用分析

目的 分析广东海风藤超临界萃取物的化学成分.方法 采用CO2超临界流体萃取广东海风藤的脂溶性部位,以气相色谱-质谱联用(GC-MS)法鉴定化学成分,面积归一化法测定各成分相对含量.结果 从广东海风藤超临界萃取物中共分离出28个组分,鉴定了其中25个化合物,占萃取物总量的78.33%,主要为T-杜松醇(18.195%)、8-杜松烯(11.485%)、α-没药醇(8.304%)和瓦伦烯(6.672%).结论 广东海风藤的挥发油提取物中主要含有萜烯和萜醇.     

四季感冒片中3味药材超临界CO_2复方萃取物挥发性成分分析

目的:分析四季感冒片中紫苏叶、陈皮、荆芥的超临界CO2复方萃取物挥发性成分。方法:采用超临界CO2萃取技术萃取四季感冒片中的3味药材的挥发性成分,采用气相色谱-质谱法对复方提取物进行成分分析。结果:超临界CO2复方提取法的提取率为2.21%,从复方萃取物中分离到21个化合物,鉴定出16个化合物,主要成分是甜橙黄酮(36.56%)和亚油酸(19.52%)。水蒸气蒸馏法提取率为1.035%,从复方提取物中共分离出51个化合物,鉴定出32种化合物,主要成分是D-柠檬烯(62.40%)和侧柏酮(15.49%)。结论:超临界CO2复方萃取技术可提取紫苏叶、陈皮、荆芥3味药材中的挥发性成分,但与水蒸气蒸馏法所得复方挥发油的成分存在差别。     

GC-MS分析不同水蒸气蒸馏法提取的莲子心挥发油成分

目的 分析比较不同水蒸气蒸馏法所得莲子心的挥发油成分。方法 分别采用水蒸气蒸馏装置(SDA)和挥发油测定装置(EODA)的水蒸气蒸馏法提取莲子心挥发油,GC-MS分离鉴定挥发油成分,峰面积归一化法计算百分含量。结果 采用SDA法,鉴定出29种成分,占挥发油总量91.56%,主要成分为棕榈酸(28.96%)、9,17-十八碳二烯醛(19.99%)和亚油酸(11.94%)等;采用EODA法,鉴定出18种成分, 占挥发油总量77.96%,主要成分为棕榈酸(18.98%)、肉桂酸龙脑酯(12.58%)、2-甲氧基-4-乙烯苯酚(8.25%)等。结论 两种水蒸气蒸馏法所得挥发油成分存在较大差异,且SDA较EODA更适合于提取挥发油。     

GC-MS分析不同水蒸气蒸馏法提取的莲子心挥发油成分

目的分析比较不同水蒸气蒸馏法所得莲子心的挥发油成分。方法分别采用水蒸气蒸馏装置（SDA）和挥发油测定装置（EODA）的水蒸气蒸馏法提取莲子心挥发油,GC-MS分离鉴定挥发油成分,峰面积归一化法计算百分含量。结果采用SDA法,鉴定出29种成分,占挥发油总量91.56%,主要成分为棕榈酸（28.96%）、9,17-十八碳二烯醛（19.99%）和亚油酸（11.94%）等;采用EODA法,鉴定出18种成分,占挥发油总量77.96%,主要成分为棕榈酸（18.98%）、肉桂酸龙脑酯（12.58%）、2-甲氧基-4-乙烯苯酚（8.25%）等。结论两种水蒸气蒸馏法所得挥发油成分存在较大差异,且SDA较EODA更适合于提取挥发油。     

药对陈皮—干姜与其单味药挥发性成分的比较分析

目的:比较分析药对陈皮-干姜与其单味药的挥发性成分.方法:采用水蒸气蒸馏法分别提取陈皮,干姜药材及药对挥发性成分,应用气相色谱-质谱联用(GC-MS)技术对各样品中的挥发性成分进行比较分析,并采用峰面积归一化法计算百分含量.结果:从陈皮挥发性成分中检出的4-异丙基甲苯、D-柠檬烯、壬醛、大根香叶烯等成分和干姜挥发性成分中检出的甲基庚烯酮、α-法尼烯、5-甲基-2-(1-甲基乙烯基)-4-己烯-1-醇乙醇酯、α-长叶蒎烯等成分在药对挥发油中均未检出;而药对陈皮-干姜中新增成分冰片、2-甲基丙酸-3,7-二甲基-2,6-辛二醇酯、β-桉叶醇、肉桂苯氨基甲酸酯等.结论:药对陈皮-干姜配伍后挥发性化学成分与单味药相比有明显差异.     

中药酸枣仁的化学成分研究

目的：研究酸枣仁的化学成分。方法：采用乙醇提取,硅胶、SephadexLH-20柱色谱等方法分离纯化,根据理化性质和波谱方法鉴定化合物的结构。结果：从酸枣仁中分离得到7个化合物,分别鉴定为豆甾4-烯-3-酮（Ⅰ）、苯丙氨酸（Ⅱ）、甘油（Ⅲ）、异当药黄素（Ⅳ）、正二十六酸（Ⅴ）、槲皮素（Ⅵ）、齐墩果酸（Ⅶ）。结论：化合物Ⅴ～Ⅶ为首次从该植物中分离得到。     

广陈皮的超临界流体萃取和水蒸气蒸馏挥发油的比较分析

目的:比较两种不同提取方法所得的广陈皮挥发油的挥发性化学成分。方法:分别采用超临界CO2流体萃取(SFE)和水蒸气蒸馏(SD)的方法提取广陈皮的挥发油。运用气相色谱-质谱联用法分离和分析两挥发油的挥发性化学成分,主要成分棕榈酸和D-柠檬烯采用标准品的峰面积增大法进一步确认。结果:从广陈皮SFE和SD挥发油中共鉴定出22个成分,占色谱总流出峰面积的97%以上,两者的提取率分别为5.05%和0.46%。SFE挥发油的主要成分为挥发性较弱、相对分子量较大的棕榈酸,SD挥发油的主要成分为挥发性较强、相对分子量较小的D-柠檬烯。此外,SFE和SD挥发油中均有含量不低的2-甲胺基-苯甲酸甲酯。结论:采用两种方法提取广陈皮所得挥发油的挥发性成分不尽相同,且SFE法的提取率高于SD法;两种方法均能将广陈皮的特征性成分2-甲胺基-苯甲酸甲酯提取出来。     

脱氟阿托伐他汀钙的全合成

目的:全合成得到脱氟阿托伐他汀钙,为阿托伐他汀产品质量分析及控制提供重要依据。方法:以异丁酰乙酸乙酯为起始原料,通过胺解,缩合,M ichael-Stetter反应,Paal-Knorr反应,得到关键中间体化合物7,再经酸性条件脱保护及碱性条件酯水解成钠盐,最后与醋酸钙成钙盐得到目标化合物脱氟阿托伐他汀钙。结果:目标化合物结构经1H-NMR、ESI-MS确证。结论:通过该法全合成得到了脱氟阿托伐他汀钙,对阿托伐他汀质量指标的控制具有重要参考价值。     

Synthesis, analgesic, anti-inflammatory and antibacterial activities of some novel 2-methyl-3-substituted quinazolin-4-(3H)-ones

A series of novel 2-methyl-3-substituted quinazolin-4-(3H)-ones have been synthesized by treating (2-methyl-4-oxo-3H-quinazolin-3-yl)dithiocarbamic acid methyl ester with different amines, the starting material dithiocarbamate was synthesized from anthranilic acid. The compounds synthesized were investigated for analgesic, anti-inflammatory and antibacterial activities. All the test compounds exhibited significant activity, the compounds VA2, VA3 and VA4 shown more potent analgesic activity, and the compounds VA3 and VA4 shown more potent anti-inflammatory activity than the reference compound diclofinac sodium.     

Analysis of prostaglandins in aqueous solutions by supercritical fluid extraction and chromatography

Trace amounts of prostaglandins (PGs) were selectively analysed without derivatization using supercritical fluid extraction (SFE) and open tubular column supercritical fluid chromatography (SFC). The specific compounds studied were prostaglandin F2 alpha (PGF2 alpha), esters of PGF2 alpha, prostaglandin F1 alpha) and prostaglandin E2 (PGE2). An open tubular column was used with carbon dioxide as the mobile phase and with universal flame ionization detection. Samples were introduced into the column by direct injection using a 1-microliter sample loop or by SFE with solute focusing. The 11 standard compounds were effectively separated within 35 min using a density program at constant temperature. The minimum detectable quantity (signal-to-noise ratio = 3) using the direct injection method was 9 ng for 15-propionate PGF2 alpha isopropyl ester. Using the extraction method, the sample size in the extraction cell was increased to 100 microliters, which made it possible to analyse compounds that were present in low concentrations. Aqueous PG samples were extracted from adsorbents onto which the samples had been loaded.     

超临界CO2萃取分析苏合香的化学成分

目的分析苏合香挥发油的化学成分。方法采用超临界CO2法提取苏合香挥发油,并通过气相色谱-质谱(GC-MS)联用技术,分析鉴定其中的化学成分。结果通过计算机检索,鉴定了其中的73个化合物,占挥发油色谱峰总面积的87%。主要成分为苄基肉桂酸(2.53%)、苯甲酸苄酯(29.87%)、乙酸苄酯(1.71%)、乙酰苯丙酯(1.83%)、石竹烯(2.42%)、肉桂酸异丁酯(3.05%)、绿叶烯(1.81%)、去氢自莒烯(1.04%)、硬尾醇氧化物(1.71%)、17-氧白羽扇豆碱(2.80%)、脱氢-4-上松香醇(5.20%)、2-葵基十六烷基脱氢-[2,1-a]茚(3.06%)等。检出成分占挥发油总量的71%。结论所用方法为苏合香的合理利用提供了科学依据。     

The application of supercritical fluid extraction to cocaine and its metabolites in blood and urine

Supercritical fluid extraction (SFE) is emerging as a valuable analytical technique for use as an alternative to conventional solid-phase (SPE) and liquid-liquid extraction techniques. It is a relatively new technique based on the use of supercritical fluids for the isolation of analytes from various matrices and is attracting great interest because of the increasing need for a simple, rapid, environmentally friendly, automated, and selective extraction method. A new method using SFE procedures for the extraction of cocaine and its major metabolites, benzoylecgonine and ecgonine methyl ester, from whole blood and urine was developed. This study has shown that cocaine and its metabolites can be successfully extracted from blood and urine using SFE techniques. Levels measured using SFE have shown analyte recovery better than 70% for cocaine, better than 40% for benzoylecgonine, and better than 85% for ecognine methyl ester from whole blood and urine. Good run-to-run reproducibility was observed between each extraction with limits of detection and quantitation of 1 ng and 10 ng based on 200 microL of blood and urine. A comparison between SPE and developed SFE techniques was investigated to observe if a correlation existed between the two methods. Studies proved that a correlation did exist between the two methods for spiked blood and urine samples with comparative results. This paper details a procedure for the extraction of cocaine and its metabolites from blood and urine.     

Optimization and comparison of three methods for extraction of volatile compounds from Cyperus rotundus evaluated by gas chromatography-mass spectrometry

The essential oil of Cyperus rotundus has multiple pharmacological activities. Therefore, the extraction with high yield and quality is very important for preparation of essential oil of C. rotundus. In this paper, three methods, namely hydrodistillation (HD), pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE), for extraction of volatile compounds from C. rotundus were optimized and compared by gas chromatography-mass spectrometry. Among eight identified compounds in C. rotundus, five components including alpha-copaene, cyperene, beta-selinene, beta-cyperone and alpha-cyperone were quantitatively determined or estimated using alpha-cyperone as standard, which showed that PLE had the highest extraction efficiency, while SFE had the best selectivity for extraction of beta-cyperone and alpha-cyperone. The contents of ingredients from C. rotundus extracted with HD, PLE and SFE are significantly different, which suggest that comparison of chemical components and pharmacological activities of different extracts is helpful to elucidate the active components in C. rotundus and control its quality.     

Synthesis and structural characterization of derivatives of 2- and 3-benzo[b]furan carboxylic acids with potential cytotoxic activity

Derivatives of 2- and 3-benzo[b]furancarboxylic acids were prepared and evaluated for their cytotoxic potential in the National Cancer Institute, Bethesda, USA. Six compounds: 7-acetyl-6-hydroxy-3-methyl-2-benzofurancarboxylic acid (2), 6-hydroxy-7-(p-methoxycinnamoyl)-3-methyl-2-benzofurancarboxylic acid (4), 5-bromo-7-hydroxy-6-methoxy-2-benzofurancarboxylic acid methyl ester (6a), 6-acetyl-5-(O-ethyl-2'-diethylamino)-2-methyl-3-benzofurancarboxylic acid methyl ester (1f), 6-(O-ethyl-2'-diethylamino)-7-p-methoxycinnamoyl)-3-methyl-2-benzofurancarboxylic acid methyl ester hydrochloride (4b), 5-bromo-7-(O-ethyl-2'-diethylamino)-6-methoxy-2-benzofurancarboxylic acid methyl ester (6b) showed significant cytotoxic activities against human cancer cell lines. In addition the crystal structures of 7-methoxy-2-benzofurancarboxylic acid methyl ester (7a) has been solved by X-ray structure analysis of single crystals.     

植物内生真菌HCCB00189代谢产物研究

目的：研究植物内生真菌HCCB00189的代谢产物。方法：采用溶剂萃取、硅胶柱层析及制备HPLC等方法，对活性菌株的发酵物进行分离，并根据理化性质和光谱分析对化学结构进行鉴定。结果：从其代谢产物中分离到5个化合物，鉴定为4-甲基苯甲酸羧甲基酯（1）；4-甲氧甲酰基苯甲酸（2）；4-羟甲基苯甲酸（3）；4’，7-二羟基异黄酮（4）和4’，5，7-三羟基异黄酮（5）。抗肿瘤活性测试表明化合物4，5对肿瘤细胞有较明显的抑制作用。结论：从植物内生真菌HCCB00189代谢产物中分离到抗肿瘤活性成分。     

气-质联用分析比较麻黄及其炮制品中挥发性成分(英文)

采用气质联用法分析麻黄生品及其炮制品种的挥发油成分。采取水蒸汽蒸馏法和超临界流体萃取技术提取麻黄各品种中的挥发油, 其中通过水蒸汽蒸馏法提取得到的麻黄生品、蜜麻黄和清炒麻黄挥发油中, 鉴定的成分分别为48, 57和48种, 蜜炙和清炒后分别产生14 和 9种新成分通过超临界流体萃取法提取得到的麻黄生品、蜜麻黄和清炒麻黄挥发油中, 鉴定的成分分别为22, 36和28 种, 蜜炙和清炒后分别产生15 和23种新成分。麻黄经炮制后挥发油成分和相对含量均发生了明显变化, 这可能是导致麻黄炮制品功效的改变原因之一。