燕子掌挥发油化学成分的研究

应用气象色谱-质谱联用技术对燕子掌挥发油化学成分进行了分析研究,共鉴定出66种组分与燕子掌主要挥发性化学成分以苯乙醇、2,6,6-三甲基-2,4-环庚二烯-1-酮、6,10,14-三甲基十五烷-2-酮、十六烷酸甲酯、十六烷酸乙酯、十八烷酸甲酯为主要成分,化合物类型以酮、酯、类等化合物为主,其中十六烷酸甲酯的含量最高,占挥发油总量的26．13％。     

棉蚜和茉莉酸甲酯诱导棉花挥发物组分分析

采用固相微萃取和气质联用技术,对健康棉叶、蚜害棉叶、蚜害棉叶-棉蚜复合物、茉莉酸甲酯处理棉叶以及棉蚜蜜露和棉蚜自身挥发物成分进行了提取和组分分析。共检测出27种挥发性化学物质。健康棉叶、蚜害棉叶、蚜害棉叶-棉蚜复合物、茉莉酸甲酯处理棉叶挥发物中,均含α-蒎烯、β-蒎烯、β-石竹烯、十五烷、十六烷、十七烷、-Cyclohexen-1-ol,1-(1,5-dimethyl-4-hexenyl)-4-methyl-7种组份。蚜害棉叶或蚜害棉叶-棉蚜复合物中检测到α-水芹烯、α-石竹烯、α-法尼烯、2,6,10-三甲基十五烷、(E,Z)-2,6-二甲基-2,4,6-辛三烯、2,6,10,14-四甲基十五烷、蒽、二酚基丙烷8种组份;3-蒈烯、(E)-β-法尼烯只在蚜害棉叶及茉莉酸甲酯处理棉叶中被检测出。在棉蚜及其蜜露中都能检查到壬醛、癸醛、十四烷、十五烷、十六烷、十七烷;而1-甲氧基-4-[(Z)-1-丙烯基]苯、(E)-β-法尼烯、菲只在棉蚜蜜露中被检查到;6,10-二甲基-5,9-十一双烯-2-酮只在棉蚜中被检测到。研究结果为进一步开展棉花、棉蚜挥发物对天敌昆虫的吸引作用研究奠定了基础。     

异色瓢虫4变种成虫对茶和茶蚜气味行为反应

用Y形嗅觉仪测定了异色瓢虫4个变种成虫对茶蚜利它素的行为反应,结果表明,供给茶蚜、甘蓝蚜和萝卜蚜的两两组合,茶蚜+蚜害茶梢和正常茶梢,蚜害茶梢和正常茶梢,天敌分别选择茶蚜、茶蚜+蚜害茶梢或蚜害茶梢(P<0.05);以8～9种质量梯度的茶蚜+蚜害茶梢、蚜害茶梢和茶蚜做味源,瓢虫对味源趋向率与味源质量呈Logistic曲线关系(P<0.01),其中二斑变型、显现变种和十九斑变种对茶蚜的趋向率与蚜数呈左偏的单峰曲线(P<0.01);茶蚜体表乙醚或正己烷漂洗物也有引诱力,以显明变种最敏感.     

华西银腊梅挥发油化学成分的研究

用水蒸气蒸馏法提取华西银腊梅挥发油,并用气相色谱-质谱(GC-MS)联用技术对其挥发油的化学成分进行分析,结果共鉴定了其中的39种成分,所鉴定成分含量约占总检出量的87.83%。其化学成分主要为(Z,Z)-9,12-十八碳二烯酸甲酯(9.00%),壬醛(5.83%),二十一烷(5.69%),二十烷(5.08%),辛炔酸(4.50%),2,6,10,15-四甲基十七烷(3.93%),(Z)-6-十八烯酸甲酯(3.65%),3,8-二甲基十一烷(3.52%),1-十六碳炔(3.31%),肉豆蔻酸(2.86%),月桂醛(2.81%),壬酸(2.23%),5,6,7,7α-四氢-4,4,7α三甲基-2(4H)-苯并呋喃酮(2.18%)等。     

半仿生法提取艾叶挥发油的研究

湖南产艾叶经过"半仿生法"(SBE)浸提-水蒸气蒸馏获得挥发油,产油率为1.05%,较直接蒸馏水浸提-水蒸气蒸馏提高0.3%.以上采用气相色谱-质谱联用仪结合标准图谱和文献分析其化学组分,半仿生法浸提的挥发油共检出33个成分,其中11个成分是直接水蒸气蒸馏获得的样品中所没有的组分,如桉树脑、薄荷酮、(-)-乙酸龙脑酯、1,3-(2-氢)-二酮-2-氨基-1氢-1-吲哚、邻苯二甲酸单乙酯、菊槐酮、顺-异丁子香酚、α-紫穗槐烯、石竹烯醇、11,15-二甲基三十五烷等,有些具有一定的研究开发价值.     

云南干巴菌挥发油化学成分的研究

利用气相色谱－质谱联用技术对云南干巴菌的挥发油化学成分进行了研究,共鉴定出49种组分。其中主要成分为业油酸甲酯、棕榈酸、1,1－二乙氧基乙烷、苯乙醛、十六碳烯酸、十五烷酸、邻苯二甲酸二丁 、苯甲酸、苯乙醇、硬脂酸、二十一烷、肉豆蔻酸、十八碳烯酰胺、苯乙酸等,其中亚油酸甲酯的含量最高,占挥发油成分总量的27.12％,检出成分占挥发油总量的90％。     

瑞香狼毒茎叶化学成分研究

新鲜瑞香狼毒（Ｓｔｅｌｅｒａｃｈａｍａｅｊａｓｍｅ）茎叶经正己烷提取,脱腊后进行ＧＣＭＳＤＳ联用分析,鉴定出２０个化合物。主要成分为正十八烷;正十九烷;２,６,１０,１４四甲基十六烷;十六烷酸;十六烷酸甲酯;十六烷酸乙酯;９,１２,１５十八碳三烯酸甲酯;９,１２十八碳二烯酸;９,１２,１５十八碳三烯酸和十八烷酸。     

福建省山苍籽果实的精油成份分析

本文报道了使用蒸馏、干柱层析、薄层层析、毛细管气相色谱、色谱-质谱联机等手段,分析了福建省几个产地的山苍籽商品精油成份,鉴定出26种成份,其中α-正丁酮、β-水芹烯、β-蒎烯、顺式-芳樟醇氧化物、反式-芳樟醇氧化物、正十一烷、α-龙脑烯、龙脑、萜品-4醇、正十二烷、胡椒酮、三甲基十二烷等12种成份,均未见报道过;对鉴定成份进行定量分析。     

木荷花挥发性成分的GC-MS分析

采用无水乙醚超声萃取得到新鲜木荷(Schima superba)花浸膏提取物,顶空固相微萃取富集挥发性成分,气相色谱-质谱联用仪分析,归一化法计算各组分的相对含量.鉴定出挥发性化合物中的51个成分,约占相对总含量的99%;挥发性成分中含氧化合物的含量超过93%,其中主要的化合物及其相对含量为酮代异佛尔酮(26.33%)、氧化芳樟醇(19.53%)、环氧芳樟醇(8.80%)、3,7-二甲基-2,6-辛二烯-1-醇(8.23%)、白藜芦素(7.89%)、4-羟基3,5,5-三甲基-2-环己烯-1-酮(6.54%)、2,6,6-三甲基-1,4-环己二酮(4.06%)、苯乙醇(2.17%)、2-甲基-2-壬烯-1-醇(2.04%)等.     

茶互利素和蚜性信息素及其组合调控大草蛉行为的效应

茶蚜群聚于茶梢上刺吸,而茶梢是加工名优茶的原料,不便施药治蚜。大草蛉虽是茶蚜主要天敌之一,但在自然情况下不足以控制茶蚜。遂探讨以茶梢互利素、蚜虫性信息素及其组合引诱大草蛉制约茶蚜的技术。使用顶空吸附法采集蚜害茶梢和健康茶梢挥发物,经GC-MS分析发现蚜害茶梢(E)-2-戊烯醛、苯甲醛和α-法尼烯的含量丰富。将蚜害茶梢挥发物中16种主要成分、蚜虫性信息素荆芥内酯和荆芥醇、以及α-法尼烯、苯甲醛和荆芥醇的2∶2∶6比例混合物分别制成味源,这19种味源的剂量都是200!g。经检测发现荆芥醇、荆芥内酯、α-法尼烯、(E)-2-戊烯醛和苯甲醛引起大草蛉的EAG值明显大于其它13种单组分引起的EAG值,而小于α-法尼烯、苯甲醛和荆芥醇混合物引起的EAG值。再将荆芥内酯和荆芥醇分别按7种比例配成7种味源,还把α-法尼烯、苯甲醛和荆芥醇的2∶2∶6比例混合物、以及(Z)-3-己烯-1-醇、(E)-2-戊烯醛、(E)-2-己烯醛、苯甲醛和α-法尼烯分别作为味源,用这13种味源分别制成的诱芯于秋季茶园中诱集大草蛉,每个诱芯含有信息物质总量是10 mg,结果表明:α-法尼烯、苯甲醛和荆芥醇混合物的诱效最强,称为大草蛉诱集剂;荆芥内酯和荆芥醇1∶9或0∶10比例的混合物诱效次之。深秋置大草蛉诱集剂诱芯于蚜群中,可诱来许多大草蛉成虫捕食茶蚜,并产卵于茶园中而增加大草蛉幼虫越冬基数,翌年春季就近捕食越冬蚜卵孵化的茶蚜。该诱集剂及其使用技术可作为一种治理茶蚜手段。     

Analysis of n-hexane, 2-hexanone, 2,5-hexanedione, and related chemicals by capillary gas chromatography and high-performance liquid chromatography

Analytical methods, using capillary gas chromatography and normal-phase high-performance liquid chromatography, were developed for the analysis of the neurotoxic chemicals n-hexane, 2-hexanone, and 2,5-hexanedione and their suspected metabolites. Two gas chromatographic methods, using a 50-m glass capillary OV 101 column and cyclohexane as an internal standard, were employed. In both methods, the injector and detector temperatures were 220 and 280 degrees C, respectively. In method I the following temperature program was used: isothermic at 50 degrees C for 30 min, followed by a temperature increase of 10 degrees C/min to a final temperature of 180 degrees C, which was then maintained for 7 min. This method was used to analyze the following compounds: n-hexane, 2,5-dimethylfuran, 2-hexanone, 3-hexanone, hexanal, 1-hexanol, 2-hexanol, 3-hexanol, 5-hydroxy-2-hexanone, gamma-valerolactone, 2,5-hexanedione, and 2,5-hexanediol. Method II, which was developed for n-hexane and eight of its more common metabolites, used the following temperature program: isothermic at 70 degrees C for 15 min, followed by a temperature increase of 40 degrees C/min to a final temperature of 220 degrees C, which was maintained for 5 min. A linear relationship between peak area and amount injected was observed over a 100-fold range. The minimum detectable amounts ranged from 0.05 to 1 microgram, depending on the compound. Normal-phase HPLC, using a 5-micron silica cartridge fitted into an RCM-100 radial-compression separation system, was utilized to analyze 2-hexanone and its metabolites 2,5-dimethylfuran, gamma-valerolactone, 5-hydroxy-2-hexanone, and 2,5-hexanedione.(ABSTRACT TRUNCATED AT 250 WORDS)     

藏药短管兔耳草挥发性化学成分的研究

采用毛细管气相色谱—质谱联用技术对藏药短管兔耳草挥发性化学成分进行了研究,经毛细管色谱分离出62个峰,共确定了其中41种化学成分,所鉴定的化合物含量占全挥发油的77．32％;用气相色谱面积归一化法测定了各化学成分的相对含量,其主要化学成分为：二苯胺(16．47％)、邻苯二甲酸丁基—8—甲基壬基酯(6．42％)、二十六碳烷(4．76％)、十六烷酸(3．66％)、二十四碳烷(3．40％)、邻苯二甲酸二丁酯(3．38％)、二十二碳烷(3．30％)、二十碳烷(3．26％)、十六烷酸乙酯(2．77％)、十八碳烷(2．76％)、戊酸(2．48％)、3—乙基环辛烯(2．05％)等。     

Composition of the volatiles from intact and tea aphid-damaged tea shoots and their allurement to several natural enemies of the tea aphid

Abstract: The comparison between the composition of the volatiles from intact tea shoots (ITS) and that from tea aphid-damaged tea shoots (TADTS) was accomplished, and the difference of both volatiles in attraction to natural enemies of the tea aphid, Toxoptera aurantii , i.e the ladybug, Leis axyridis (Pallas), the aphid parasite, Aphidius sp., and the lacewing, Chrysopa septempunctata Wesmeal, was investigated in the current paper. Volatile components from ITS, obtained by air entrainment, were identified by their mass spectra and retention times and comfirmed by comparison with authentic samples. They are E-2-hexenal, ocimene, Z-3-hexenyl acetate, Z-3-hexen-1-ol, butanoic acid-3-hexenyl ester, linalool, 1-octanol, geraniol and indole. Volatiles from TADTS have been identified as E-2-hexenal, ocimene, Z-3-hexenyl acetate, Z-3-hexen-1-ol, linalool, geraniol, indole, benzaldehyde and E-2-hexenoic acid. Z-3-hexen-1-ol is the main component in the two kinds of volatiles, whilst benzaldehyde is the another main component in TADTS volatiles. The air entrainment extracts of TADTS and benzaldehyde elicit the stronger electroantennogram (EAG) responses, and the stronger upwind flight and arresting behaviour from each natural enemy in wind tunnel. EAG responses from Leis axyridis and Chrysopa septempunctata were bigger than those from Aphidius sp., whereas Leis axyridis responds to these odours slightly less than Aphidius sp. and Chrysopa septempunctata in wind tunnel bioassay. So TADTS emits volatile synomones, in which the amount of benzaldehyde is ample and its allurement is the strongest.     

Anaerobic degradation of xenobiotics by organisms from municipal solid waste under landfilling conditions

The potential for biological transformation of 23 xenobiotic compounds by microorganisms in municipal solid waste (MSW) samples from a laboratory scale landfill reactor was studied. In addition the influence of these xenobiotic compounds on methanogenesis was investigated. All R11, 1,1 dichloroethylene, 2,4,6 trichlorophenol, dimethyl phthalate, phenol, benzoate and phthalic acid added were completely transformed during the period of incubation (> 100 days). Parts of the initially added perchloroethylene, trichloroethylene, R12, R114, diethyl phthalate, dibutyl phthalate and benzylbutyl phthalate were transformed. Methanogenesis from acetate was completely inhibited in the presence of 2,5 dichlorophenol, whereas 2,4,6 trichlorophenol and R11 showed an initial inhibition, whenafter methane formation recovered. No transformation or effect on the anaerobic microflora occurred for R13, R22, R114, 3 chlorobenzoate, 2,4,6 trichlorobenzoate, bis(2 ethyl)hexyl phthalate, diisodecyl phthalate and dinonyl phthalate. The results indicate a limited potential for degradation, of the compounds tested, by microorganisms developing in a methanogenic landfill environment as compared with other anaerobic habitats such as sewage digestor sludge and sediments.Abbreviations BBP benzylbutylphthalate - DEHP bis(2 ethylhexyl) phthalate - 3 CB 3 chlorobenzoate - R22 chlorodifluoromethane - CFC chlorofluorocarbon - R13 chlorotrifluoromethane - cis1,2 DCE cis 1,2 dichloroethylene - DBP dibutyl phthalate - R12 dichlorodifluoromethane - 1,1 DCE 1,1 dichloroethylenel - R114 dichlorotetrafluoroethane - 2,5 DCP 2,5 dichlorophenol - DEP diethyl phthalate - DiDP diisodecyl phthalate - DMP Dimethyl phthalate - DNP dinonyl phthalate - MSW dunicipal solid waste - PCE perchloroethylene - PA phthalic acid - PAE phthalic acid esters - R11 trichlorofluoromethane - 2,4,6 TCB 2,4,6 trichlorobenzoate - 2,4,6 TCP 2,4,6 trichlorophenol - VC vinylchloride     

Impairment of human polymorphonuclear leukocyte chemotaxis by 2,5-hexanedione

The effect of n-hexane metabolites on human polymorphonuclear leukocyte chemotaxis and luminol-dependent chemiluminescence was investigated. No effect was detected when 2-hexanol, 2-hexanone and -valerolactone were used, 2,5-hexanedione at 75 g/ml inhibited chemotaxis and a direct correlation between increasing the xenobiotic concentration and the degree of inhibition was found. Chemotactic peptide-induced chemiluminescence was not affected by 2,5-hexanedione. In order to clarify the phenomenon, plasma membrane fluidity was investigated by fluorescence polarization of the fluorescent probe trimethylammonium diphenylhexatriene. 2,5-hexanedione increased the membrane fluidity, while the other n-hexane metabolites did not change the degree of flourescence polarization. Results suggest that the cellular functions modulated by membrane-cytoskeletal organization are affected by 2,5-hexanedione also at the low concentrations.Abbreviations 2,5-Hxdn 2,5-hexanedione - 2-Hxl 2-hexanol - 2-Hxn 2-hexanone - PMN polymorphonuclear leukocyte - TMA DPH trimethylammonium diphenylhexatriene - -V1 -valerolactone     

Urinary 2,5 hexanedione as a biomarker of n-hexane exposure

n-Hexane is a saturated aliphatic hydrocarbon widely used in industry. In most cases it is used as a mixture with hexane isomers and various others solvents in the form of commercial hexane. n-Hexane is metabolized oxidatively to a number of compounds, including 2,5-hexanedione (2,5-HD), which is eliminated through the urine and is implicated in the neurotoxic effect of this solvent. The main objective of this study was to evaluate urinary 2,5-HD as a biomarker of n-hexane exposure. The study was carried out in seven industrial units. Post-shift urine samples from 111 workers who handled commercial hexane were collected and analysed for 2,5-HD by capillary gas chromatography. Air sampling was performed in the breathing zones of the workers, and the air samples were analysed using validated methods. Monitoring individual exposures showed that n-hexane exposure varied from 5 to 70 p.p.m. (mean±SD = 15.24±2.98 p.p.m.). Significant correlation was observed between exposure to n-hexane and urinary 2,5-HD levels, with high correlation coefficients (ρ= 0.81, p = 0.000), suggesting that urinary 2,5-HD is a good biomarker of occupational exposure to n-hexane. Urinary 2,5-HD is recommended as a better tool than air monitoring in the assessment of health risk, namely the early detection of n-hexane neurotoxicity.     

Urinary 2,5 hexanedione as a biomarker of n-hexane exposure

n-Hexane is a saturated aliphatic hydrocarbon widely used in industry. In most cases it is used as a mixture with hexane isomers and various others solvents in the form of commercial hexane. n-Hexane is metabolized oxidatively to a number of compounds, including 2,5-hexanedione (2,5-HD), which is eliminated through the urine and is implicated in the neurotoxic effect of this solvent. The main objective of this study was to evaluate urinary 2,5-HD as a biomarker of n-hexane exposure. The study was carried out in seven industrial units. Post-shift urine samples from 111 workers who handled commercial hexane were collected and analysed for 2,5-HD by capillary gas chromatography. Air sampling was performed in the breathing zones of the workers, and the air samples were analysed using validated methods. Monitoring individual exposures showed that n-hexane exposure varied from 5 to 70 p.p.m. (mean ±SD = 15.24 ±2.98 p.p.m.). Significant correlation was observed between exposure to n-hexane and urinary 2,5-HD levels, with high correlation coefficients ( ρ= 0.81, p = 0.000), suggesting that urinary 2,5-HD is a good biomarker of occupational exposure to n-hexane. Urinary 2,5-HD is recommended as a better tool than air monitoring in the assessment of health risk, namely the early detection of n-hexane neurotoxicity.     

黑藻(Hydrilla verticillata)养殖水对铜绿微囊藻(Microcystic aeruginoSa)的抑制效应及其机制

黑藻（Hydrilla verticillata）养殖水对铜绿微囊藻（Microcystic aeruginosa）的生长有明显抑制作用。同时,它显著降低铜绿微囊藻的光合速率;而使呼吸速率与超氧物歧化酶（SOD）活性先升高,后迅速下降;使细胞膜透性显著增大。电镜照片显示,黑藻养殖水对铜绿微囊藻的超微结构产生进行性的损伤,对质膜、类囊体片层及拟核区的破坏尤为显著。黑藻养殖水的乙醚提取物有显著抑制微囊藻生长的作用,且呈现明显的量效关系,证实黑藻对铜绿微囊藻的克生作用是通过向水中分泌克藻物质实现的。经GC—MS分析和初步鉴定,黑藻养殖水的乙醚提取物中含有邻苯二甲酸二异辛酯、邻苯二甲酸二丁酯、邻苯二甲酸丁酯2-甲基丙酯等物质。     

Two new reactive targets of 2,5-hexanedione in vitro – beta-alanine and glycine

Summary. In this study, we found that two amino acids reacted with 2,5-hexanedione to form new reaction products in vitro, respectively. In the reaction of beta-alanine and 2,5-hexanedione, a reaction product was obtained and analyses of obtained results showed it was 3-(2,5-dimethyl-1H-pyrrol-1-yl)propanoic acid; in the reaction of glycine and 2,5-hexanedione, a reaction product was also obtained and analyses showed it was (2,5-dimethyl-1H-pyrrol-1-yl)acetic acid. Two reaction products were found to be oxidized easily; in addition, the latter was more easily to be oxidized than the former in the air. Our discoveries demonstrated that reactions between amino acids and 2,5-hexanedione could exist possibly in vitro. At present, it is clear that 2,5-hexanedione causes either axon atrophy or swelling, but the underlying molecular mechanism is still unclear. Since both beta-alanine and glycine are considered as neurotransmitter in the central nervous system, the reaction products remain to be identified in vivo.     

Evaluation of 2,5-hexanedione in urine of workers exposed to n-hexane in Brazilian shoe factories

Urinary 2,5-hexanedione (2,5-HD) is used as a biomarker for biological monitoring of workers exposed to n-hexane. The purpose of this study was to compare two types of treatment of urine samples during clean-up (with and without acidic hydrolysis) and to study the exposure situation of workers exposed to n-hexane during shoe manufacturing. There, various glues containing n-hexane are used. Quantification of 2,5-HD was carried out by gas chromatography and flame ionization detection (GC-FID). Fifty-two urine samples taken from workers of seven shoe factories were analyzed. Thirty-four persons from the administrative staff of the same factories served as controls. They were not known to be exposed to n-hexane. The samples treated with acidic hydrolysis showed levels (average 0.94 mg/l) approximately 10 times higher than samples without acidic hydrolysis (0.09 mg/l). The difference is predominantly caused by the conversion of other metabolites of n-hexane (e.g. 4,5-dihydroxy-2-hexanone) to 2,5-HD in the presence of acids. Our results also show, that exposure to n-hexane is different between various industries. Levels of 2,5-HD in urine are predominantly dependent on the type of operation (how the glue is applied on the leather during shoe manufacturing). Simple measures, e.g. using a glue handgun instead of a paintbrush significantly decreased exposure to n-hexane.