高效液相色谱法测量青海湖浮游植物色素浓度

2003年8月，我们利用高效液相色谱法(HPLC)对浮游植物色素进行分类定量分析。结果表明青海湖的叶绿素类以叶绿素a和b为主，叶绿素a浓度最高；光合作用类胡萝卜素种类极少，浓度很低；光保护色素种类较多，浓度较高，其中以Zea，Diadino，β．β-Car和Viola为主。     

HPLC analysis of algal pigments: a comparison exercise among laboratories and recommendations for improved analytical performance

Pure individual and mixed pigment standards were distributed among Joint Global Ocean Flux Study (JGOFS) pigment analysts to estimate the variability of their spectrophotometric and chromatographic systems. To monitor the integrity of the pigments during the comparison exercise, chlorophyll and carotenoid standards were archived and periodically analyzed by high-performance liquid chromatography (HPLC). Pigment standards stored in the dark under nitrogen at − 20 °C were found to be stable for periods of at least one year. Results from three separate intercalibration exercises document a better agreement for spectrophotometric analyses than for HPLC. For the spectrophotometric comparisons, 90% of the pigments analyzed by participant laboratories were within ± 6% of the mean “consensus” values. By contrast, 65 and 85% of the laboratories agreed to within ± 10 and ± 20%, respectively, when chromatographic analyses were compared. Chlorophyll absorption measurements obtained with a diode array-type spectrophotometer were 6–9% lower than those obtained with monochromator-type spectrophotometers. These underestimates probably result from chlorophyll fluorescence contamination associated with the optical configuration of the diode array spectrophotometer. It was also determined that HPLC methods which are not capable of separating monovinyl chlorophyll a from divinyl chlorophyll a can produce 15–25% overestimates of total chlorophyll a concentration in Prochlorococcus-dominated oceanic waters. A simple dichromatic approach is described for eliminating this variable source of error caused by co-elution of these structurally-related pigments. The use of internal standards and periodic calibration checks with external standards is highly recommended for improving analytical performance.     

高效液相色谱法测量海洋浮游植物色素浓度

JGOFS计算和SeaWiFS计划推荐高效液相色谱（HPLC）作为海洋浮游植物色色浓度的测量方法。文章参考SeaWiFS计划制定的HPLC分析规范，叙述采用反相C18ODS色谱柱、996PDA、自动进样器（未配柱温箱）和三元梯度的色谱法测量海洋浮游植物色素浓度的具体实践。     

HPLC determination of phytoplankton pigments using N,N-dimethylformamide

The suitability of N,N-dimethylformamide (DMF) as an extractant for the standard reverse-phase HPLC method was examined using algal cultures. Good pigment separations and recovery were achieved with 20% (volume %) addition of an ion-pairing solution in an injection. While slight amounts of degradation products of chlorophylla, i.e., chlorophyllidea, allomeric and epimeric forms, were produced, adequate attention to filtration and extraction prevents the formation of degradation products, confining them to an acceptable level. Because of its strong extractability, which expedites the extraction process, DMF is an efficient solvent for HPLC analysis of phytoplankton pigments.     

基于反相C8色谱柱的海洋浮游藻色素高效液相色谱分析方法有效性验证

对一种海洋浮游藻色素高效液相色谱分析方法进行了有效性验证。该方法使用反相C8色谱柱,以甲醇、乙腈和丙酮为流动相,并在流动相中添加吡啶/醋酸溶液作为修饰剂改善色素峰的分离效果。结果表明,4种色素标准在一定的浓度范围内线性关系良好,叶绿素a的线性范围为189.6~18 960μg/L,叶绿素b为89.2~8 920μg/L,β,β-胡萝卜素为7.77~777.2μg/L,叶黄素为15.28~1 528μg/L。除β,β-胡萝卜素外各色素标准的回收率在不同浓度下均在90%以上,相对标准偏差也普遍低于5%。在4个参考藻种和123个胶州湾现场样品中共检测出37种色素,一些关键的特征色素均获得了良好的分离效果。该方法操作简便,具有分离度好、灵敏度高、重复性好、回收率高等优点,适用于培养的藻种和现场样品中的海洋浮游藻色素分析。     

An automated computational method for planing hull form definition in concept design

This paper describes the development of a computer-based method for producing chined planing boat hull forms adequate to be applied in concept design. The method is based on a principle where the designer specifies a small set of critical parameters he/she wishes obtain or keep preserved and generates a complete hull form, without the traditional skilled recourse of giving stations point by point. From this set of parameters a detailed and faired drawing with offsets is generated very quickly. The method allows, in its execution mode, the flexibility to modify, adjust and enlarge the input set of parameters. The method was created to allow both (1) automated hull form definitions when integrated to an existing computer system and (2) quick but detailed preliminary calculations of stability, lift and drag, volumes and internal space allocations, sea-keeping estimates, etc., all with very reasonable precision. As application examples some planing boat hull forms are generated. Some are typical and others less usual. The later ones are defined to show the method's limits, in order to validate it.     

番红砗磲外套膜色素提取条件优化及成分分析

以番红砗磲(Tridacna crocea)为实验对象,通过单因素对比实验对其外套膜色素的提取条件进行了优化,并利用薄层层析色谱法对色素组成进行了初步分析。结果表明:丙酮和乙醇为适宜的番红砗磲外套膜色素提取剂;使用丙酮为提取剂时,浸提时间为4 h,提取温度为25℃,料液比为1︰40。使用乙醇为提取剂时,浸提时间为4 h,提取温度为30℃,料液比为1︰200;利用薄层色谱法分离外套膜颜色为蓝色和红棕色的番红砗磲外套膜色素后发现,蓝色番红砗磲外套膜色素由9种色素组分构成,红棕色个体番红砗磲外套膜色素由10种色素组分构成。     

Effects of iron and humic acid on competition between Microcystis aeruginosa and Scenedesmus obliquus revealed by HPLC analysis of pigments

Iron is a vital micronutrient for growth of bloom-forming Microcystis aeruginosa and competition with other algae, and its availability is affected by humic aci...     

甲壳胺寡糖的液相色谱及薄层层析分析

为了解低分子甲壳胺多糖的抗肿瘤辅助疗效,作者利用高效液相色谱法(HPLC)结合薄层色谱法(TLC),探讨了SUGAR-KS-802寡糖分析柱分析甲壳胺寡糖的条件,并尝试了几种薄层层析展开剂对甲壳胺寡糖组分的展层条件。结果表明,在HPLC流动相为0．001mol／L NaOH溶液,流速0．2mL／min时,可将混合的标准甲壳胺寡糖成分很好地分离;采用乙酸乙脂：甲醇：水：氨水=5：9：1：1．5混合液作为硅胶薄板展开剂时,可将不同聚合度的甲壳胺寡糖很好地分开,且层析重现性高,糖残基数目和Rf值具有很好的线性关系。2种分析方法结合可以作为1种可靠的甲壳胺寡糖分析方法。     

Application of an automated method for dissolved sulphate analysis to marine and brackish waters

A fully automated method for the analysis of dissolved sulphate was tested for saline and brackish waters. A small sample volume of ? 2 ml is required, making the method very suitable for analysis of interstitial waters. The method was calibrated for samples from natural waters in the Dutch delta region, containing up to 2500 mg l^?1 of sulphate, and with a salinity of 30‰.     

低硫酸化杂多糖水解单糖高效液相色谱指纹图谱研究

低硫酸化杂多糖(UF)是从海洋褐藻中分离的一种单糖组成复杂的硫酸化杂多糖,在细胞和动物实验中均表现出显著的神经保护活性,对帕金森病具有显著作用。本研究采用水提-醇沉-DEAE-Sepharose Fast Flow交换层析柱制备UF,经三氟乙酸(TFA)水解和1-苯基-3-甲基-5吡唑啉酮(1-phenyl-3-methyl-5-pyrazalone,PMP)衍生化,通过对水解条件、衍生化试剂使用量、衍生时间的考察,确定最佳衍生条件,通过高效液相色谱(HPLC)法测定UF的单糖组成,并建立UF的指纹图谱。在UF水解单糖的指纹图谱中,共标示出8个特征共有峰,经鉴别主要色谱峰8个,分别是D-甘露糖、D-甘露糖醛酸、L-鼠李糖、D-葡萄糖醛酸、D-葡萄糖、D-半乳糖、D-木糖及L-岩藻糖,其中岩藻糖含量最高,其次是半乳糖。该方法操作简便、快速、灵敏度高、重复性好,可作为UF检查和鉴别的方法,建立实验室UF质量控制标准,为临床用UF质量标准的建立奠定基础。     

An automated photochemical method for the determination of dissolved organic carbon in sea and estuarine waters

An improved version of Ehrhardt's (1969) method for the analysis of dissolved organic carbon is described. The method, which is automated, determines the carbon dioxide with a non-dispersive infra-red analyser. The conditions of photo-oxidation have been examined in order to achieve maximum performance. It was found that careful attention needed to be paid to U-V source, “oxygen source”, pH and time or irradiation. The completeness of the method was examined by three independent procedures. We concluded that in all cases the extent of oxidation of organic material was in excess of 98%. Typical performance figures were: precision ±2.5% above 2.0 mg C l^?1, approaching 0.03 mg C l^?1 below 1.0 mg Cl^?1; blank, equivalent to 0.3 mg C l^?1; sampling frequency, 10 samples per hour. The lower limit of sensitivity is mainly governed by the blank. The upper limit of the method is greater than 40 mg C l^?1.A wholly continuous modification of the method has been devised which permits on line analyses. An attentuated version of the method has been used for the analysis of total carbonate.The present and other published methods for the analysis of dissolved organic carbon in natural waters are discussed in relation to one another.     

流动注射Ferene分光光度法测定海水中溶解态铁的方法优化

热液流体中溶解态铁是海水原位测量的重要参数之一。本研究采用Ferene分光光度法,搭建流动注射分析系统,优化进样条件、显色条件,实现了热液流体中溶解态铁的在线测定。结果表明,测定Fe(II)时,Ferene、缓冲液浓度分别为8×10–3、0.4 mol/L,Ferene、样品流速分别为0.8、0.6 m L/min,显色盘管长度为40 cm时,方法的灵敏度、检测限最佳;测定Fe(III)时,Ferene、缓冲液、抗坏血酸浓度分别为1×10–2、0.5、0.01 mol/L,Ferene/抗坏血酸、样品流速均为1.0 m L/min,还原、显色盘管长度均为40 cm时,方法的灵敏度、检测限最佳。最佳实验条件下,Fe(II)、Fe(III)在0.2~10μmol/L和0.5~16μmol/L范围内,工作曲线回归方程分别为A=0.0834 C+0.0564(μmol/L,n=8,R2=0.997)和A=0.0478C+0.0423(μmol/L,n=8,R2=0.997)。Fe(II)、Fe(III)检测限分别为24、39 nmol/L,相对标准偏差分别为0.8%、1.2%(n=10),加标回收率为97.9%~103.0%。共存离子实验表明,流体中的Na+、Mn2+、Cu2+、Cu+不会对测量造成干扰。     

Short-time scale variation of phytoplankton succession in Lisbon bay (Portugal) as revealed by microscopy cell counts and HPLC pigment analysis

The phytoplankton distribution and composition in Lisbon bay was studied, at a short time scale based on a weekly sampling, during one year (April 2004 – May 2005), using microscopic examination and pigment analysis with high-performance liquid chromatography (HPLC). This work is a contribution to the knowledge on species succession and ecology of coastal communities. The frequency of the sampling permitted monitoring peak blooming and decaying, a process which frequently occurred within 1 –2 weeks.     

An FDTD method for analysis of scattering from rough fluid-fluidinterfaces

A finite-difference time-domain (FDTD) method for scattering by one-dimensional, rough fluid-fluid interfaces is presented, modifications to the traditional FDTD algorithm are implemented which yield greater accuracy at lower computational cost. These modifications include use of a conformal technique, in which the grid conforms locally to the interface, and a correction for the numerical dispersion inherent to the FDTD algorithm, Numerical results are presented for fluid-fluid cases modeling water-sediment interfaces. Two different roughness spectra, the single-scale Gaussian roughness spectrum and a multiscale modified power-law spectrum, are used. The Gaussian results are calculated as a function of the dimensionless parameters kh and kl, where k is the wavenumber in water, h is the rms surface height, and l is the surface correlation length. For the modified power-law spectrum, statistical parameters consistent with an insonification frequency of 7.5 kHz are used. Results are compared with those obtained using an integral equation technique both for scattering from single-surface realizations and for Monte Carlo averages of scattering from an ensemble of surface realizations. Scattering strengths are calculated as a function of scattering angle for an incident angle of 70° (20° grazing). The results agree well over all scattering angles for the cases examined     

基于遥感反射比光谱的一种藻类识别方法

利用所得的甲藻门和硅藻门的17种藻类遥感反射比光谱,对其进行平滑、取倒数和归一化等预处理后,进行了四阶微分处理.根据聚类分析结果,甲藻门各藻种分为一类,而硅藻门的藻种分为另一类,这说明经上述处理后,甲藻门和硅藻门的差异性显著增大.将甲藻门和硅藻门的四阶微分光谱分别平均得到门类的特征光谱,并在原始数据中加入泥沙进行敏感性...     

表征赤潮水体太阳激发的叶绿素荧光高度的波段优化 --归一化荧光高度法

采用现场实测和室内培养两种方式测定了甲藻、赤潮异弯藻、叉角藻、海洋蓝绿藻等赤潮和新月菱形藻、叉鞭金藻、塔胞藻、扁藻和小球藻等非赤潮藻类光谱曲线.采用度量太阳激发的叶绿素荧光峰高度的归一化荧光高度法,建立了不同藻类归一化荧光高度与叶绿素浓度的关系.荧光高度计算方法是将红光波段的反射率最大值(R_maxred)和R₆₈₅分别归一化到560 nm处的R₅₆₀和560 nm附近整个光谱曲线的最大值R_{560 max}上或675 nm处的R₆₇₅和675 nm附近的最小值R_675mini上.结果表明,不同藻类的R_maxred/R₅₆₀max和R_maxred/R_675mini与叶绿素a的相关系数分别比R₆₈₅/R₅₆₀和R₆₈₅/R₆₇₅与叶绿素的相关系数高,但在海洋现场测量中由于近岸二类水体其他水色组分以及大气校正误差的影响,R_maxred/R_675mini和R₆₈₅/R₆₇₅更适合于实测的叶绿素浓度估算.采用三种统计回归方程建立了不同藻类归一化荧光高度与叶绿素浓度关系,除个别藻种外,大部分的相关系数在0.9以上,其中FLH=a+(Chla)b回归方程得到的相关系数优于其他两种方法,相关系数大于0.93,这表明藻类水体的荧光特性和叶绿素浓度之间的普遍关系是非线性的.     

HPLC法同步检测鲤鱼、对虾中喹乙醇与MQCA残留

建立了一种高效液相色谱法同时检测鲤鱼、对虾肌肉组织中喹乙醇（OLA）及其代谢物3-甲基-喹啉-2-羧酸（MQCA）的残留。采用0.3 mol/L 盐酸提取鲤鱼、对虾中的残留物, C18 固相萃取柱净化, 氮气吹干及流动相定容后, Waters2695 高效液相色谱仪在320 nm（MQCA）和372 nm（QLA）双波...     

An inverse method for underwater bottom topography by using SAR imagery

I~IOXThe image technology of the synthetic aperture radar (SAR) is one of most important advances in spaceberne microwave remote sensing (Larson et al., 1976). It has extensive application in the ocean remote sensing, such as inversion of the sea subdue winds and currentS, reconstruction of underwater hatom topography and so on. Owing tO the high conductivity of sea water, an electromagnetic wave actually cannot penetrate into the sea water, with extremely smallPenetration depth (abbot 1 c…