红树植物秋茄树叶挥发油化学组成特点的气相色谱/质谱分析

用水蒸汽蒸馏法提取出秋茄树Kandelia candel叶的挥发油,经气相色谱／质谱联机分析,分离出49个峰,鉴定出35种化合物,主要是2,6-二叔丁基-4-甲基苯酚、大根香叶烯-D、十七烷、石竹烯、十九烷、十五烷、贝壳杉-16-烯等,占总峰面积的93,77％。还讨论了上述挥发油化学组成的特点及主要组分的用途。     

冷胁迫下红树植物白骨壤和桐花树叶片热值的变化

对九龙江口不同土壤盐度的白骨壤和桐花树离体叶片进行1－2℃冷胁迫处理，结果表明，随着冷胁迫时间的延长，白骨壤和桐花树叶片的热值逐渐下降，电解质渗出率呈现不同程度的上升，其中土壤盐度高的澳头白骨壤和桐花树叶片的变化幅度较土壤盐度低的白骨壤和桐花树小。白骨壤和桐花树叶片总含水量在冷处理过程中变化不大，但其自由水含量呈显著下降趋势，而束缚水含量及束缚水与自由水含量的比值则呈显著上升趋势。还原糖、可溶性糖和淀粉含量在冷胁迫过程中逐渐下降，蔗糖含量则逐渐上升。土壤盐度高的澳头白骨壤和桐花树叶片的自由水和束缚水含量的变化幅度大于土壤盐度低者，而还原糖、蔗糖、可溶性糖和淀粉含量的变幅则小于土壤盐度低者。     

红树植物白骨壤叶片衰老过程中叶肉细胞Ca2+水平的变化

用焦锑酸钙沉淀的电镜细胞化学方法，研究了白骨壤叶片衰老过程中叶肉细胞Ca^2 水平的变化．结果表明，在白骨壤幼叶和成熟叶叶肉细胞中，焦锑酸钙沉淀颗粒大量出现在液池和细胞间隙中，细胞壁中也可见少量沉淀，而细胞基质中则看不到焦锑酸钙沉淀．在衰老叶中，细胞基质和细胞膜上焦锑酸钙沉淀增加，而液泡和细胞间隙中的锑酸钙沉淀则显著减少，并且叶绿体外膜部分破损，结构破坏，核膜与液泡膜内部结构模糊，叶绿素含量、净光合速率、气扎手率和蒸腾速率显著下降．Ca^2 的区域性分布的变化与植物叶片衰老密切相关。     

红树植物木榄叶中挥发油的化学成分

以正己烷为溶剂,采用回流提取法提取红树植物木榄叶中的挥发油,运用毛细管气相色谱-质谱联用技术分离检测得到40个峰,鉴定了其中的32种成分,被鉴定成分占挥发油总量的91.92%,其主要成分为烷烃类(30.31%)、萜类化合物(25.22%)、芳香化合物(14.07%)、酸(10.60%)、酯(5.36%)和烯(3.49%).     

皱纹盘鲍脂肪酸及脂肪醛二甲基缩醛的气相色谱/质谱分析

研究了用气相色谱/质谱法测定皱纹盘鲍中脂肪酸及脂肪醛二甲基缩醛的方法。皱纹盘鲍经Folch法提取总脂,用10%硫酸-甲醇溶液进行反应,通过气相色谱/质谱法对其脂肪酸及脂肪醛二甲基缩醛的组成进行分析。实验结果表明:10%硫酸-甲醇溶液能有效地对脂肪酸进行甲酯化衍生;同时促使烯醚键断裂,并与甲醇发生缩醛反应生成脂肪醛二甲基缩醛。通过气相色谱/质谱分析,从皱纹盘鲍中共鉴定出32个化合物,包括26种脂肪酸和6种脂肪醛二甲基缩醛;脂肪酸以C16:0、C20:4(n-6)、C20:5(n-3)、C18:1(n-7)和C22:5(n-3)为主;脂肪醛二甲基缩醛以C18:0DMA和C20:1DMA为主。皱纹盘鲍肌肉和内脏中的脂肪酸及脂肪醛二甲基缩醛的组成基本一致,但内脏中的4,8,12-三甲基十三烷酸含量远高于肌肉,具有极显著差异(P<0.01)。     

黑海参脂肪酸的气相色谱/质谱法分析

黑海参(Holothuria atra)体壁经Folch 法提取总脂, 用HCl-甲醇进行甲酯化处理, 以气相色谱/质谱法分析总脂中的脂肪酸组成。从黑海参中共分析出28 种化合物, 包括25 种脂肪酸甲酯和3 种脂肪醛二甲基缩醛。黑海参体壁中的饱和脂肪酸含量为22.93%, 以C_16:0(5.49%)和C_18:0(4.38%)为主; 不饱和脂肪酸含量为65.19%, 其中单不饱和脂肪酸33.86%, 主要为C_20:1(n-9)(15.90%); 多不饱和脂肪酸为31.33%, 主要为C_20:4(n-6)(19.57%)和C_20:5(n-3)(5.86%)。脂肪醛二甲基缩醛含量为7.28%, 表明黑海参体壁总脂中含有较丰富的缩醛型甘油酯。     

五种红树植物原位根系小分子多酚组成及含量分析

红树植物的化感作用和生态功能与其多酚类物质的组成和含量密切相关,其植物根系中含有的小分子多酚对红树植物对根际生物群落的调控具有重要的意义,但对其根系中具体含有的多酚类最小单体尚缺少科学实验证据。对湛江红树林国家级自然保护区内五种重要建群红树植物进行原位根系采样,采用液相高效色谱法(HPLC)对5种主要的小分子多酚单体进行定性和定量分析。主要结果为:五种红树根系内均检测出5种小分子多酚单体,浓度含量范围在0.0007—1.7424 mg/g DW。红树植物单株含量最高值分别为,儿茶素1.7424 mg/g DW,棓儿茶素1.1470 mg/g DW,表棓儿茶素0.4457 mg/g DW,没食子酸0.2374 mg/g DW,表儿茶素0.3331 mg/g DW。5种小分子多酚含量的总平均值以秋茄(Kandelia candel)和低潮带桐花树(Aegiceras corniculatum)最高,分别为0.2778 mg/g DW、0.2379 mg/g DW。木榄(Bruguiera gymnorrhiza)和无瓣海桑(Sonneratia apetala)次之,依次为0.0766 mg/g DW、0.0734 mg/g DW。红海榄(Rhizophora stylosa)和高潮带桐花树(A.corniculatum)相对最低,分别为0.0488 mg/g DW、0.0341 mg/g DW。     

黑海参脂肪酸的气相色谱／质谱法分析

黑海参（Holothuria atra）体壁经Folch法提取总脂,用HCl-甲醇进行甲酯化处理,以气相色谱／质谱法分析总脂中的脂肪酸组成。从黑海参中共分析出28种化合物,包括25种脂肪酸甲酯和3种脂肪醛二甲基缩醛。黑海参体壁中的饱和脂肪酸含量为22．93％,以C16：0（5．49％）和C18：0（4．38％）为主;不...     

气相色谱质谱联用及电喷雾质谱法分析多棘海盘车的脑苷脂结构

通过硅胶柱层析法分离得到多棘海盘车脑苷脂,并采用气相色谱质谱联用(GC-MS)及电喷雾质谱(ESI-MS)分析鉴定其结构。GC-MS分析表明,多棘海盘车脑苷脂AAC-1、AAC-2的糖基组成相同,均为葡萄糖;长链碱主要由d18∶2、d18∶3以及少量的d22∶1组成;两者结构最主要的差别在脂肪酸部分,AAC-1由C2位不含羟基的脂肪酸组成,而AAC-2则由C2位含1个羟基取代的脂肪酸组成。ESI-MS分析结果表明,AAC-1和AAC-2的分子量范围在740～850amu之间。通过GC-MS和ESI-MS结合使用,可快速推测出多棘海盘车脑苷脂基本结构及单体分子组成,对下一步的构效关系研究具有重要意义。     

药用红树林植物黄槿的化学成分研究

利用正相硅胶柱色谱、反相硅胶柱色谱、凝胶Sephadex LH-20柱色谱、制备薄层色谱（PTLC）及重结晶等分离手段,从海洋红树林植物黄槿（Hibiscus tilisceus）中分离得到11个化合物,通过MS、1D和2D NMR等波谱技术鉴定了所有化合物的结构,分别为coniferaldehyde（1）,3,4-二羟基苯甲酸甲酯（2）,松脂醇（3）,丁香脂素（4）,格榄酮（5）,黄芪苷（6）,植醇（7）,胆甾-5-烯-3β,7α-二醇（8）,胆甾-5-烯-3β,7β-二醇（9）,胆甾醇（10）和声-胡萝卜苷（11）。这些化合物均为首次从该植物中分离获得。     

海洋红树林植物木榄化学成分研究

采用多种柱层析方法从红树植物木榄(Bruguiera gymnorrhiza(L.)Lam.)中分离获得9个单体成分,综合运用现代波谱技术鉴定了所有成分的化学结构,分别为格榄酮(I)、槲皮素-3-O-β-D-吡喃葡萄糖苷(II)、黄芪苷(III)、芦丁(IV)、3-O-甲基槲皮素(V)、羽扇豆醇(VI)、羽扇豆酮(VII)、蒲公英赛酮(VIII)和胡萝卜苷(IX),其中化合物II~V为首次从木榄属植物中分离得到。     

Determination of ammonium regeneration rates in the oligotrophic ocean by gas chromatography/mass spectrometry

A method has been developed for the determination of ammonium concentration and isotopic enrichment in seawater samples at the low nanomolar range (10–100 nmol/kg). It is based on the reaction of phenol/hypochlorite with ammonium to form indophenol, with subsequent solid phase extraction, derivatisation and analysis by Gas Chromatography Mass Spectrometry. The precision of the method was maximised by incorporating a deuterated indophenol internal standard. A system was developed which generated seawater with extremely low ammonium concentrations thus matching sample and standard matrices for quantitative analysis. Data are presented from a study of ammonium regeneration rates at three stations in the oligotrophic North–East Atlantic where ambient ammonium concentrations were < 21 nmol/kg. Results suggested that ammonium availability for phytoplankton was limited by the rate of ammonium regeneration. Efficient ammonium assimilation contributed to the very low ambient ammonium concentrations measured at these stations. The study highlights the need for the accurate determination of ammonium regeneration rates in studies of new production, particularly in extreme oligotrophic conditions. If not corrected for isotope dilution, f-ratio estimates may be overestimated by 10.7–13.7%.     

A method for the determination of nitrification rates in oligotrophic marine seawater by gas chromatography/mass spectrometry

An isotope dilution method has been developed to determine by gas chromatography/mass spectrometry (GC/MS) the rates of ammonium and nitrite oxidation in severely oligotrophic marine waters. The method is based on the formation of sudan-1 from nitrite, or from nitrate following reduction to nitrite. Samples were collected by solid phase extraction and purified by high performance liquid chromatography (HPLC). A deuterated sudan-1 internal standard was synthesized, purified by HPLC and used for quantitative analysis. Concentrations of NO₂⁻ and NO₃⁻ were generally < 2 nmol/kg and < 5 nmol/kg respectively, typical of oligotrophic surface waters, and turnover times for the inorganic N pools ranged from < 1 day to > 10 days. Significant rates of nitrification were measured in the surface oligotrophic ocean, with rates of ammonium and nitrite oxidation generally within the range of 10–500 pmol/kg/h. Consequently, a significant proportion of daily NO₃⁻ assimilation by marine phytoplankton is regenerated, and not new. In a case study of the oligotrophic gyre of the North Atlantic, the influence of NH₄⁺ regeneration and nitrification on f-ratio values suggests that in the oligotrophic ocean, f-ratio values may be significantly, and sometimes grossly, overestimated.     

Analysis of lignin-derived phenols in standard reference materials and ocean dissolved organic matter by gas chromatography/tandem mass spectrometry

A series of reference materials are proposed for intercomparison and quality control purposes during the quantification of lignin oxidation products (LOP) from diverse environmental matrices. These materials are all easily accessible and certified for diverse organic constituents (NIST and IHSS). They represent a suite of natural environmental matrices (from solids to aqueous) and are characterized by a wide range of organic carbon and lignin concentrations with abundant proportions of all major LOP. The variability of LOP concentrations and signatures for all these materials averages 3–5% and does not exceed 10%. Using these standards, a new quantification method was developed and validated for the determination of low-level CuO oxidation products using capillary gas chromatography–tandem mass spectrometry (GC/MS–MS). Tandem mass spectrometry provides both the high sensitivity and selectivity required for the identification and quantification of trace levels of dissolved lignin. The method is particularly useful for removing interference from co-eluting isotopes generated from the DOM matrix and during glucose amendment procedures of low-carbon samples. Such glucose amendment is not necessary, however, when the CuO to organic carbon weight-to-weight ratio can be kept at a value < 200–300.     

Gas chromatography and gas chromatography/mass spectrometry applied to the determination of a new pathway of pristane degradation by a marine mixed bacterial population

Degradation of pristane is rapidly achieved with high efficiency by a mixed bacterial population isolated from a marine biotope highly polluted with hydrocarbons.Analysis of the degradation products by gas chromatography and gas chromatography/mass spectrometry reveals that pristane is not only attacked according to classical mechanisms of β- and ω-oxidation, but also according to a new mechanism beginning with attack at the third carbon atom.Thanks to that mechanism, the population must be particularly suited to degradation of substrates resistant to α- and β-oxidations; this has been confirmed with an α-disubstituted structure.     

Rates of microbial degradation of petroleum components as determined by computerized capillary gas chromatography and computerized mass spectrometry

The biodegradation rates of Arabian light crude oil components under the action of a marine mixed microbial culture were monitored in a quasicontinuous culture during a 60 day experiment. The saturated hydrocarbons were degraded more rapidly and extensively (74%) than the aromatics (50%), whereas the biodegradation of asphaltenes (30%) and of resins (< 5%) was very low. The joint use of computerized high-resolution chromatography and of computerized mass spectrometry permitted classification of the petroleum constituents according to their biodegradability: (i) highly susceptible, − and iso-alkanes; (ii) susceptible, 6, 1, 5 and 2 ring alkanes, 1 ring and sulphur aromatics; (iii) moderately susceptible, 3 and 4 ring alkanes, 2 and 3 ring aromatics; (iv) resistant, tetra-aromatics, steranes, triterpanes, naphtheno-aromatics; and (v) highly resistent, penta-aromatics, asphaltenes and resins. Unlike saturates, aromatics were degraded at a rate that was in relation to the number of rings of the molecules. The microbial activity leads to the formation of a residue which can be considered as a form of stable organic matter. The biodegradation potential of a mixed microflora is much more elevated in continuous culture systems than in batch cultures.