超临界CO_2萃取连翘挥发油的正交试验和GC-MS分析

采用正交试验法对超临界CO2萃取连翘挥发油的条件进行了研究；结果显示最佳萃取条件为萃取压力30MPa，萃取温度35℃，解析压力6．7MPa，解析温度50℃，粉碎度0．55mm；按对结果的影响大小依次排列为萃取温度，粉碎度，萃取压力，解析压力，解析温度；用气相色谱－质谱联用技术测定了最佳萃取条件所得连翘挥发油的化学成分，从中鉴定出21种成分，并测定了其相对含量，主要成分为α－蒎烯、β－蒎烯、萜品醇－4、α－萜品醇、苯甲醇等。     

GC-O-MS法对酒花中香气活性成分的分析

采用顶空固相微萃取气相色谱-嗅闻-质谱((HS-SPME-GC-O-MS)联用的方法研究酒花中的香气化合物的组成和风味,并与传统的同时蒸馏萃取、水蒸气蒸馏方法进行比较,定性采用质谱谱库检索结合保留指数进行验证。结果表明:3种方法测得的1号酒花中的香气活性成分存在较大的差异,HS-SPME法最为适合,该法共鉴定出71种成分,占总峰面积质量分数的97.93%,以月桂烯、β-石竹烯为主要成分的萜烯类化合物共22种,其质量分数达88.73%,醇类及酯类质量分数分别为1.98%,3.42%。采用该方法对3个不同的酒花品种定性并嗅闻,能够嗅闻到的香气活性成分共计34种,包括碳氢化合物(包括萜烯)类7种,醇(酚)类11种,酯类10种,酮类2种,未知化合物4种。嗅闻结果表明,在1号、2号、3号3种酒花中分别嗅闻到了26,23,16种香气物质,其中重要的香气活性成分为β-香茅醇、β-石竹烯、里那醇、香叶醇、α-萜品醇、β-香茅醇、橙花醇、橙花椒醇、香叶酸甲酯、辛酸甲酯、乙酸香叶酯等。     

湘西金银花挥发油化学成分研究

采用ＧＣ／ＭＳ／ＤＳ联用仪对湘西金角花挥发油中的化学成分进行了研究。并鉴定出４０种组分。其主要成分为：芳樟醇、环氧芳樟醇、α－萜品醇、顺－３－已 烯醇、顺芷酸－３、己烯酯、香叶醇、氧化芳樟醇、法尼醇、顺－苯酮、法尼烯、大根香叶烯、橙花醇等。其中芳樟醇含量最高,约占精油总量的２０％。     

山楂挥发性化合物的气相色谱-质谱分析

采用蒸馏－萃取法收集山楂果的挥发性化合物,通过气相色谱及气相色谱／质谱分析,鉴定了３２种化合物,占总峰面积的６１％～６８％。其中主要的１０种化合物是顺－３－己烯醇、顺－３－乙酸己烯酯、α－萜品醇、糠醛、己醇、乙酸己酯、壬醛、柠檬醛、３－戊烯－２－酮,反－２－癸烯醛等。     

四方蒿精油的化学成分研究

］用HRGC和GC-MS分析了云南西双版纳的四方蒿精油的化学成分。鉴定了包括各种单萜和倍半萜的34种化合物。含量大于4的有龙脑、-蒎烯、松油烯、芳樟醇、樟烯、乙酸龙脑酯、水芹烯和18-桉叶素等8种,其中主要成分18-桉叶素达27.6四方蒿中18-桉叶素的量非常接近于河南产的木香薷中的18-桉叶素的量28.28。结果表明,香薷属中含氧单环萜型化合物也存在于中国南方的香薷。     

用极微弱化学发光法评价萜类化合物的稳定性

在60℃氧气中,用极微弱化学发光法测定单萜类化合物的化学发光强度,通过化学发光强度评价了单萜类化合物对氧气的稳定性。萜烯类化合物的稳定顺序为:γ-松油烯<莰烯<异松油烯=α-松油烯<β-蒎烯<β-月桂烯<α-蒎烯=柠檬烯。萜醇类化合物的稳定顺序为:桃金娘醇<紫苏醇<α-松油醇<龙脑=香茅醇=薄荷醇。萜醛类化合物的稳定顺序为:桃金娘醛<紫苏醛。具有同样骨骼,不同官能团的单萜类化合物稳定顺序为:萜醛<萜醇<萜烯。     

薰衣草精油化学成分的研究

〕用气相色谱和色--质谱联用从国产薰衣草油（197号）中鉴定出六十八种化合物,甲基乙烯基酮、2-甲基丙烯醛、5-已烯-2-酮、3,3-二甲基戊烷、1-甲基-2-异丙基苯、7-辛烯-4-醇、2-辛烯-4-醇、蒲勒酮、月桂烯醇、顺式－香苇醇、柠檬醛-b、胡椒酮、香树烯、萜品二醇水合物、a-葎草烯、榧素和绿叶烷是首次在薰衣草油中被发现。使用OV-17的高效玻璃毛细管柱（SCOT柱）在分析中获得满意的结果。     

头花杜鹃挥发油化学成分的研究

应用分馏、硅胶柱层析和含硝酸银的氧化铝柱层析,从头花杜鹃发油中分得24个化合物,经紫外光谱、红外光谱、核磁共振谱、质谱及气相色谱的测定,其中20个化合物被鉴定为:d-α-蒎烯(1),dl-JB-蒎烯(2),香叶烯(3),顺式-α-罗勒烯(4),β-古芸烯(5),δ-杜松烯(6),γ-芹子烯(7),α-芹子烯(8),χ-芹子烯(9),反式β-法呢烯(10),α-葎草烯(11),(一)-16α-贝壳杉醇(12),醋酸冰片酯(13),α-萜品醇-4(14),α-萜品醇(15),反式松油醇(16),里哪醇(17),前异水昌蒲二醇(18),环氧薇草烯-Ⅱ(19)和桧脑(20). 化合物4,5,11～17和19是首次从杜鹃属植物中分到.     

酸催化环合合成△~(1,8)-5,5-双甲基-六氢-7-氧代-萘-2-乙酸甲酯

近年来一些2位含氧的萜类化合物引起了人们的兴趣,虽已报道一些2位含氧的三环三烯萜的合成,但化合物2-oxo-(?)nt-manool     

α-萜品烯马来酰亚氨基酰腙化合物合成及抑菌、除草活性研究

以α-萜品烯(1)为原料,与马来酸酐反应,通过Diels-Alder环加成得到α-萜品烯马来酸酐(2),再与水合肼酰化得到中间体N-氨基-α-萜品烯马来酰亚胺(3),然后在冰醋酸的催化下分别与多氟取代苯甲醛发生缩合反应,合成了9个多氟α-萜品烯马来酰亚胺基酰腙4a～4i。通过傅立叶变换-红外光谱(FT-IR)、核磁共振(~1H NMR和~(13)C NMR)以及电喷雾-质谱(ESI-MS)等多种手段对目标化合物进行结构表征。初步的抑菌活性测试表明,在质量浓度50 mg·L~(-1)下,化合物3-三氟甲基-α-萜品烯马来酰亚氨基酰腙(4b),2,4-二氟-α-萜品烯马来酰亚氨基酰腙(4e),2,5-二氟-α-萜品烯马来酰亚氨基酰腙(4f),3,4-二氟-α-萜品烯马来酰亚氨基酰腙(4h),对苹果轮纹病毒抑制率分别为93.9%,75.5%,70.1%,75.4%;除草活性测试表明:在质量浓度100 mg·L~(-1),3-三氟甲基-α-萜品烯马来酰亚氨基酰腙(4b),4-三氟甲基-α-萜品烯马来酰亚氨基酰腙(4c)对油菜的胚根生长具有的抑制作用分别为62.2%,48.2%。综合分析,在质量浓度100 mg·L~(-1)下,化合物3-三氟甲基-α-萜品烯马来酰亚氨基酰腙(4b)的综合效果最好,对苹果轮纹病菌抑制率93.9%,活性级别为A级,对油菜的胚根生长的抑制率62.6%,活性级别为B级。     

The identification of new ATAD2 bromodomain inhibitors: the application of combined ligand and structure-based virtual screening

Ligand-based virtual screening (LBVS) and structure-based virtual screening (SBVS) approaches were used to identify new inhibitors for ATAD2 bromodomain. The LBVS approach was used to search 23,129,083 clean compounds to identify compounds similar to an active compound with reported pIC₅₀ equal to 7.2. Based on LBVS results, 19 compounds were selected. To perform SBVS, by applying nine filters on 23,129,083 clean compounds, 1,057,060 compounds were selected. After performing SBVS on these selected compounds with idock software, 16 compounds with the lowest binding energies were selected. More accurate molecular docking analysis was performed on these 35 selected compounds by using iGEMDOCK software and six of them with the lowest binding energies were selected as hit compounds. These compounds were zinc36647229, zinc77969074, zinc13637358, zinc77971540, zinc12991296 and zinc19374204.     

二维网状结构超分子化合物[Cu(dafo)2(H2O)2](Cl04)2的两种同分异构体的合成与表征

用4，5—二氮芴-9-酮（dafo）、邻苯二甲酸、高氯酸铜和4，5—二氯芴—9— 酮(dafo)、苯甲酸、高氯酸铜进行混和反应时分别得到亮蓝色和蓝绿色晶体，它们 的结构通过单晶X射线衍射法测定。其单晶结构表明，这两种化合物是同分异构体 ，组成都是C22H16Cl2CuN4O12。这两种化合物是通过氢键形成的具有二维网状结构 的超分子化合物，并通过元素分析、红外光谱、热分析对两种化合物进行了表征。     

Gas chromatography-olfactometry analysis of the volatile compounds of two commercial Irish beef meats

The volatile flavour compounds of two commercial Irish beef meats (labelled as conventional and organic) were evaluated by gas chromatography-olfactometry and were identified by gas chromatography-mass spectrometry. The volatile compounds were isolated in a model mouth system. Gas chromatography-olfactometry was performed by a group of eight assessors using the detection frequency methodology. The odours of the detected compounds were described as well. Eighty-one volatile compounds were identified, 11 compounds of which possessed odour activity in the first beef sample and 14 of which in the second meat sample. Ten volatile flavour compounds were common to both: methanethiol, dimethyl sulphide, 2-butanone, ethyl acetate, 2- and 3-methylbutanal, an unknown compound, 2-octanone, decanal and benzothiazole. Two unknown compounds were only detected in the first sample while 2,3-pentanedione, 4-methyl-3-penten-2-one, 2-heptanone, dimethyl trisulphide and nonanal were only perceived in the second beef. Significant differences in terms of detection frequency, odour characteristics and in nature of the volatile flavour compounds were emphasised between the two samples.     

硝基苯并咪唑衍生物的合成、表征及抑菌活性的测定

以苯并咪唑为原料,经硝化、二茂铁磺酰化等步骤,合成了8种未见文献报道的硝基苯并咪唑衍生物,其结构经MS,¹H NMR和元素分析确证.由于硝基苯并咪唑的互变异构,二茂铁磺酰化后,产生两个异构体,用X射线衍射仪测定了化合物2a的晶体结构.初步的抑菌实验结果表明,该系列化合物具有良好的抑菌作用,其抑菌活性均优于对照药剂50%多菌灵可湿性粉剂.     

One step synthesis of azo compounds from nitroaromatics and anilines

A general and efficient method for synthesis of both symmetric and asymmetric aromatic azo compounds in one single step has been developed. The nitro compounds were reduced and the substituted anilines were oxidized by each other without any metal in the base condition. Various azo compounds with halogen, methyl and methoxy functional group were obtained by using available, cheap nitro compounds and substituted anilines. In addition, the electronic effect and substituent effect of the compounds have been discussed.     

宝明页岩柴油碱性氮化物的梯度富集及GC-MS分析

利用溶剂萃取和柱色谱等技术浓缩分离新疆宝明页岩油柴油馏分中的碱性氮化物。以宝明页岩柴油为原料,经糠醛溶剂精制,初步得到富集碱性氮化物的抽出油。以抽出油为深度富集碱性氮化物的原料,采用柱色谱等分离方法,从抽出油中分离得到碱性氮化物。利用傅立叶变换红外光谱仪(FT-IR)和气相色谱-质谱联用仪(GC-MS)分别对富集的碱性氮化物进行官能团检测和定性、定量分析。结果表明:新疆宝明页岩油柴油馏分中的碱性氮化物经溶剂精制和柱色谱等分离方法梯度富集后,碱性氮化物的质量分数由抽出油的12.08%提高到最终产物的69.48%,并在富集分离的产物中鉴定出60种碱性氮化物,其中主要为苯胺类、喹啉类和吡啶类化合物,各占25.85%,23.56%和16.52%。     

异色满酮-4及其衍生物的合成IX异香豆素并杂环化合物的合成

本文通过3, 4-二氢异苯并吡喃酮-4和其β-二酮衍生物的缩合反应, 合成出3, 4-二氢异苯并吡喃并吲哚、并喹啉、并吡唑和并嘧啶类化合物, 并进一步氧化成标题化合物。所合成的新化合物均经核磁共振光谱红外光谱及元素分析证明其分子结构。     

GC-MS of volatile components of Schisandra chinensis obtained by supercritical fluid and conventional extraction

In this paper, the volatile compounds of Schisandra chinensis obtained by different extraction techniques including supercritical fluid extraction (SFE), steam distillation (SD), Soxhlet extraction (SE) and ultrasound-assisted extraction (UAE) were investigated for the first time. The sample preparation procedure for GC-MS analysis of the volatile compounds was optimized and then 37, 45, 27 and 37 compounds were identified in the samples obtained by SFE, SD, SE and UAE methods, respectively. As the therapeutic effect of the traditional Chinese medicine is usually based on multifarious essential components or the combination of them instead of only one component, the volatile compounds were compared in groups with the extracts by SE, SD and UAE. This would be more reasonable to evaluate the effects of an alternative technique to extracting multifarious essential components. Among the identified components in the SFE extract, 32 compounds were the same as that by three conventional methods, accounting for 90.5% of the volatile compounds identified. However, as the volatile compounds were classed into groups, it was easy to see that the Schisandra chinensis oil extracted by SFE was made up largely of aromatics and sesquiterpenoids (52.1 and 27.6%, respectively), with less amounts of monoterpenoids and other compounds, distinguishing SFE from the conventional extractions.     

Effect of γ-irradiation on volatile compounds of dried Welsh onion (Allium fistulosum L.)

The volatile compounds of γ-irradiated dried Welsh onion were isolated by simultaneous distillation–extraction (SDE) technique and then analyzed by gas chromatography–mass spectrometry (GC–MS) along with their non-irradiated counterparts. A total of 35 volatile compounds were identified in non-irradiated and 1 kGy irradiated samples and 36 volatile compounds were identified in 3, 5, 10 and 20 kGy irradiated samples so far belong to chemical classes of acid, alcohol, aldehyde, ester, furan, ketone and S-containing compound. S-containing compounds were detected as major volatile compounds of all experimental samples. Though the content of several compounds was increased after irradiation, content of major S-containing compounds was found to decreased in the process. Application of high-dose irradiation if required for microbial decontamination of dried Welsh onion is feasible as it enhanced the total concentration of volatile compounds by 31.60% and 24.85% at 10 and 20 kGy, respectively.     

N-取代芳环-4-氨基喹唑啉类化合物的合成及生物活性研究

以4-氯喹唑啉和芳香胺反应,合成了三个新的N-取代苯环或杂环4-氨基喹唑啉类化合物.三个新化合物经1HNMR,IR及元素分析证明其结构.生物活性测试表明,三个新化合物均有一定的抑菌效果.