海水中多氯联苯的气相色谱分析方法

本文叙述了用于测定天然海水中多氯联苯的气相色谱分析方法,本法采用国产1300(1)型树脂提取富集天然海水中PCB_s,在2000ml空白海水中添加100ng PCB₅/l,让其通过树脂柱,树脂柱对多氯联苯的平均富集效率为87.4%样品提取液通过微型硅胶混合层析柱,旨在净化与分离经与同类的分析方法比较,本方法使用有机溶剂及固体吸附剂用量少,既经济、省时,又可降低分析过程的试剂空白值。本方法用普通氮气代替K-D浓缩器浓缩样品提取液,操作简便快速。用2000ml空白海水与2000ml天然海水分别添加25-125ng PCB₅/l的标准溶液,让外加标准的海水样品通过分析全过程,其平均回收率在66-73%,变异系数在±10%之内,试验结果表明,本方法适于测定表层海水中ng/l级的多氯联苯。     

基于指纹图谱和含量测定评价脑得生丸的质量

目的：以高效液相色谱(HPLC)指纹图谱结合含量测定方法,为科学评价脑得生丸的质量提供理论依据。方法：采用HPLC建立脑得生丸的指纹图谱,色谱柱为 Inertsil ODS-SP（4.6 mm×250 mm,5μm）;流动相为乙腈-0.1%甲酸溶液,梯度洗脱;柱温 30℃;检测波长为254 nm;流速为1 ml/min。采用HPLC方法测定脑得生丸中人参皂苷 Rg1,色谱柱为 HypersilODS2（4.6 mm×250 mm,5μm）;流动相为乙腈-0.05%磷酸（19∶81）,等度洗脱;检测波长为 203 nm;流速为 1.0 ml/min;进样量为10 μl。基于指纹图谱和含量测定结果,对脑得生丸的质量进行评价。结果：建立了脑得生丸的指纹图谱,确定了11个共有峰,15批脑得生丸样品相似度均大于0.97。人参皂苷 Rg1的线性方程为 y=13600x-9.5581,线性范围是 19.2 μg/ml～1.920 mg/ml,相关系数是0.9992。15批脑得生丸中有5批样品为过期产品,仅批次为161003样品（过期5个月）含量检测不合格,其他均符合质量标准要求。结论：该方法简便、准确、重复性好,为脑得生丸质量的有效评价与整体控制提供了实验依据。     

液相色谱要原子荧光联用测定海水中无机砷和有机砷

本文研究并建立了海水中测定砷形态的液相色谱—原子荧光法。进行了实验参数流动相浓度、pH、流速的优化。在优化的实验条件下,采用Hamilton PRP-X100分析柱在6 min内可以完成三价砷、甲基砷和五价砷3种形态的分离、检测。在载流5% HCl,还原剂2% KBH4、0.5% KOH,进样量100 μL的条件下,三价砷、甲基砷和五价砷的检出限分别为0.31 μg/L、0.52 μg/L和0.36 μg/L。在浓度2~80 μg/L范围内,3种砷形态均有良好的线性关系,相关系数均优于0.999。用本文所建立的方法进行了海水样品中无机砷和有机砷形态的测试,海水中三价砷、甲基砷的含量较低,五价砷稍高,说明海水中砷形态主要以五价砷存在,当加标量为5~10 μg/L,加标回收率在73%~104%之间。该方法操作前处理简单,灵敏度高、运行费用低廉,适用于海水中砷形态的测试。     

液相色谱—原子荧光联用测定海水中无机砷和有机砷

本文研究并建立了海水中测定砷形态的液相色谱—原子荧光法,进行了实验参数流动相浓度、pH、流速的优化。在优化的实验条件下,采用Hamilton PRP-X100分析柱在6 min内可以完成三价砷、甲基砷和五价砷3种形态的分离、检测。在载流5%HCl,还原剂2%KBH4和0.5%KOH,进样量100μL条件下,三价砷、甲基砷和五价砷检出限分别为0.31μg/L、0.52μg/L和0.36μg/L。在浓度2～80μg/L范围内,3种砷形态均有良好的线性关系,相关系数均优于0.999。用本文所建立的方法进行了海水样品中无机砷和有机砷形态的测试,海水中三价砷、甲基砷的含量较低,五价砷稍高,说明海水中砷形态主要以五价砷存在,当加标量为5～10μg/L时,加标回收率在73%～104%之间。该方法操作前处理简单,灵敏度高、运行费用低廉,适用于海水中砷形态的测试。     

离线固相萃取螯合富集分离-ICP-MS测定海水中的稀土元素

通过测定条件优化、方法比对等实验建立了一种固相萃取小柱离线螯合富集分离电感耦合等离子体质谱仪测定海水中稀土元素的方法。海水样品通过调节p H后,进入VAC ELUT SPS24 Agilent圆形固相萃取装置,其主要基体物质的去除率高于97%;萃取富集的优化条件是海水样品p H 4.0~7.0,海水进入萃取柱速率2 m L/min,硝酸洗脱液浓度为1 mol/L;方法对稀土元素的加标回收率为83%~108%,14种稀土元素的检出限为0.057~0.613 ng/L,RSD10%;该方法与氢氧化铁共沉淀法富集稀土元素比对测定结果一致,方法具有准确度与精密度高、操作简便快速等优点,可用于海水样品中稀土元素的定量精确测量。     

HPLC法测定宁志胶囊中芒果苷含量的研究

目的：建立测定宁志胶囊中芒果苷含量的HPLC法。方法：采用高效液相色谱法,色谱柱为Agilent 5TC-C₁₈（250 mm×4.6 mm,5 μm）,以乙腈-0.2%冰醋酸溶液（13∶87）为流动相,检测波长为258 nm,流速为1.0 ml/min,柱温为30 ℃。结果：芒果苷在4.0951～51.1885 μg/ml之间呈良好线性关系（r=0.99987）。芒果苷平均加样回收率为104.92%（n=6）,RSD=1.20%。结论：经方法学验证,本法可用于宁志胶囊的质量控制。     

海水中微量氰化物的气相色谱测定法

本文介绍了一种海水中微量氰化物的气相色谱测定法。取10ml清洁水样,用稀醋酸将pH调节至6—7,加入磷酸缓冲液,混合均匀后,加入0.25ml 1％氯胺T,水中的氰化物转变为氯化氰,以还原剂除去剩余氧化剂后,用乙醚萃取分层,直接取样进行色谱测定。本方法快速简便,易于操作,且灵敏度高,最低检出浓度可达0.5μg/L。该法已用于青岛胶州湾沿岸表县水中氰化物的测定,并与海洋污染调查规范法进行过对照实验。     

颗粒与饮片浸膏制备的滋阴温阳活血膏方临床用量一致性研究

目的：通过测定指标性成分含量,比较配方颗粒和全方药材浸膏制备的滋阴温阳活血膏方的临床等效用量之间的差异。方法：含量测定采用高效液相色谱（HPLC）法,使用Phenomex Kinetex C_{18色谱柱（4.6mm×250mm,5μm）,0.1%磷酸-乙腈为流动相,梯度洗脱,流速1.0ml/min,柱温30℃,进样量10μl,检测波长254nm;以腺苷和山奈酚-3-O-β-D-葡萄糖苷为指标性成分,共测定颗粒和浸膏配制的膏方各10批。结果：10批样品中,1g颗粒制备的膏方相当于0.957～1.043g浸膏制备的膏方,二者差异无统计学意义（P＞0.05）。结论：使用配方颗粒可以替代药材浸膏作为制作膏方的材料。}     

HPLC法同时测定滋阴温阳活血颗粒中两种指标性成分的研究

目的：建立滋阴温阳活血颗粒中两种指标性成分（腺苷和山奈酚-3-O-β-D-葡萄糖苷）的同时测定方法。方法：采用HPLC法,选用phenomex Kinetex C_{18色谱柱（4.6mm×250mm,5μm）,0.1%磷酸-乙腈为流动相,梯度洗脱,流速1.0ml/min,柱温30℃,进样量10μm,检测波长254nm;以腺苷和山奈酚-3-O-β-D-葡萄糖苷为指标性成分,共测定10批滋阴温阳活血颗粒。结果：10批颗粒中,腺苷的含量在2.706～4.132mg/g范围内,山奈酚-3-O-β-D-葡萄糖苷的含量在3.692～4.948mg/g范围内。结论：本研究所建立方法快速、准确、高效,能够对滋阴温阳活血颗粒的质量进行科学评价。}     

地黄活血汤调控IL-6表达治疗子宫平滑肌瘤活性成分的筛选和测定

目的：筛选并准确测定地黄活血汤调控白细胞介素（IL）-6表达治疗子宫平滑肌瘤的活性成分,作为其基于功效的质量评价指标。方法：活性筛选采用酶联免疫吸附（ELISA）法,分别加入地黄活血汤中所含各成分单体,测定其对IL-6表达的影响,将产生显著影响者列入候选;以上述候选成分为指标,进行高效液相色谱法（HPLC）含量测定研究,使用Waters Xbridge C18色谱柱（4.6 mm×250 mm,5 μm）,乙腈-0.2%磷酸为流动相,梯度洗脱,流速1.0 ml/min,检测波长254 nm,柱温30℃,进样量10 μl;选择毛蕊花糖苷、木通皂苷D为指标性成分,共测定10批药材制备的供试品溶液。结果：ELISA法检测出毛蕊花糖苷、木通皂苷D、川续断皂苷乙、表儿茶素、芍药苷具有较为显著的IL-6表达调控活性;含量测定结果表明,毛蕊花糖苷、木通皂苷D在地黄活血汤中含量分别为0.0370～0.0534 mg/ml和0.0419～0.0590 mg/ml。结论：地黄活血汤中的毛蕊花糖苷、木通皂苷D能体外抑制IL-6的表达,建议列为该方基于功效主治的质量控制指标成分。     

Microbial Biomass and Organic Nutrients in the Deep-Sea Sediments of the Central Indian Ocean Basin

In order to assess the impact of deep-sea mining on the in situ benthic life, we measured the microbial standing stock and concentration of organic nutrients in the deep-sea sediments of the Central Indian Ocean Basin in the Indian pioneer area. Sediments were collected using box core and grab samples during September 1996. The total bacterial numbers ranged from 10 10 -10 11 cells per g -1 dry weight sediment. There was a marginal decrease in the number of bacteria from surface to 30 cm depth, though the subsurface section registered a higher number than did the surface. The highest numbers were encountered at depths of 4-8 cm. The retrievable number of bacteria were two orders less in comparison with the direct total counts of bacteria. An almost homogeneous distribution of bacteria, total organic carbon, living biomass, and lipids throughout the depth of cores indicates active microbial and benthic processes in the deep sea sediments. On the other hand, a uniform distribution of total counts of bacteria, carbohydrates, and total organic carbon in all the cores indicates their stable nature and suggests that they can serve as useful parameters for long-term monitoring of the area after the benthic disturbance. Further studies on temporal variability in this region would not only verify the observed norms of distribution of these variables but would also help to understand restabilization processes after the simulated benthic disturbance.     

海上大直径钢管桩打桩过程中桩周土强度弱化研究

海上大直径钢管桩打桩过程中,桩周土体受到强烈扰动而发生强度弱化,掌握桩周土体强度弱化规律对于准确预测打桩过程、保证工程安全具有重要意义。为研究土体强度弱化规律,开展了环剪试验模拟打桩对桩周土体的扰动,测试土体强度随剪切速率的变化规律,建立了描述土体强度弱化规律的拟合公式,引入到打桩分析软件中。研究结果表明：土体的强度折减程度不仅与土体本身的性质有关还受到土体的埋深和剪切速率的影响,埋深越深土体强度折减程度越低,剪切速率越高土体强度折减越高,在打桩分析中可采用这里推荐的线性折减方法来模拟不同深度处土体强度的折减规律。     

Geoacoustic Inversion via Genetic Algorithm and Its Application to Manganese Sediment Identification

An acoustic inversion method using a wide-band signal and two near field receivers is proposed and applied to multiple layered seabed models including a manganese sediment. The inversion problem can be formulated into a probabilistic model comprised of signals, a forward model, and additive noise. The forward model simulates wide-band signals, such as chirp signals, and is chosen to be the source-waveletconvolution plane wave modeling method. The wavelet matching technique, using weighted least-squares fitting, estimates the sediment sound-speed and thickness on which determination of the possible numerical ranges for a priori uniform distribution is based. The genetic algorithm is applied to a global optimization problem to find a maximum a posteriori solution for determined a priori search space. Here the object function is defined by an L 2 norm of the difference between measured and modeled signals. Not only the marginal pdf but also its statistics are calculated by numerical evaluation of integrals using the samples selected during importance sampling process of the genetic algorithm.     

Phylogenetic diversity and phenotypic characterization of cultivable bacterioplankton isolated from polar oceans

A set of 27 marine planktonic bacteria isolated from the polar regions was characterized by 16S rDNA sequencing and physiological and biochemical testing. More than half of these bacteria were positive for caseinase, gelatinase and 13-glucosidase, and could utilize glucose, maltose or malic acid as carbon source for cell growth. Twelve isolates expressed nitrate reduction activities. Except for one antarctic isolate BSwlO175 belonging to Actinobacteria phylum, these isolates were classified as γ-Proteobacteria, suggesting that γ-Proteobacteria dominated in cultivable marine bacterioplankton at both poles. Genus Pseudoalteromonas was the predominant group in the Chukchi Sea and the Bering Sea, and genus ShewaneUa dominated in cultivable bacterioplankton in the Prydz Bay. With sequence similarities above 97%, genus Psychrobacter was found at both poles. These 27 isolates were psychrotolerant, and significant 16S rDNA sequence similarities were found not only between arctic and antarctic marine bacteria （ 〉 99% ）, but also between polar marine bacteria and bacteria from other aquatic environments （ ≥ 98.8% ）, including temperate ocean, deep sea, pond and lake, suggesting that in the polar oceans less temperature-sensitive bacteria may be cosmopolitan and have a bipolar, even global, distribution at the species level.     

Deep-Sea Sediment Compression Curves: Some Controlling Factors, Spurious Overconsolidation, Predictions, and Geophysical Reproduction

Oedometer tests have been carried out on 70 undisturbed surficial clays (at approximately 250 mm below the mudline), mostly collected by free-fall corers from sites widely scattered throughout the deep-sea North Atlantic. Acoustic measurements were also made, initially on contiguous samples and ultimately on the same sample using a geophysically instrumented oedometer which also collected electrical resistivity data. Apart from those quiescent areas below the carbonate compensation depth, such as north of the West Indies where very fine clays exist, most of the samples are silty clays whose geotechnical-geophysical properties are dependent on the type of clay minerals present (and their ability to take in moisture), the sand-size fraction, and the quantity of carbonate present. Thus the pure clays have high compressibilities which decrease on the addition of coarse particles, while the converse is true for the acoustic parameters, these increasing with the sand fraction. Using the notion of the intrinsic compression line for all samples, and comparison to it of the measured compression curves, it is clear that, contrary to some previously held ideas, most deep-sea clays are normally consolidated; the addition of carbonate has the effect of creating an open, stronger sediment skeleton. Interestingly, where information is available, the variation with depth of a sample's acoustic velocity follows the void ratio pressure relationship of the compression curve. This allows the construction of an in-situ sediment compression curve using the in-situ geophysical observations.     

INFORMATION FOR AUTHORS

<正>Acta Oceanologica Sinica(AOS)is a comprehensive academic journal edited by the Editorial Committee of Acta Oceanologica Sinica and is designed to provide a forum for important research papers of the marine scientific community which reflect the information on a worldwide basis.The journal publishes scholarly papers on marine science and technology,including physics,chemistry,biology,     

Estimation of Sediment Properties during Benthic Impact Experiments

Sediment properties, such as water content and density, have been used to estimate the dry and wet weights, as well as the volume of sediment recovered and discharged, during benthic impact experiments conducted in the Pacific and Indian Oceans. The estimates show that the weights of dry (355-1332 t) and wet sediment (1651-4888 t) recovered during the experiments, are not only a function of the total duration and distance covered during the experiment, but also depend on water content and density of the sediment. Estimation of dry sediment and its volumetric ratio in the discharge, are key parameters for calculating the discharged volume. The estimated volume of wet sediment recovered (1427-4049 m 3 ) as well as discharged (2693-6951 m 3 ) during the experiments, provide important inputs to evaluate the sediment resettlement and migration. Using these estimates, the average depth of excavation on the seafloor, can also been calculated. However, the stages of sediment recovery and discharge are expressed differently in some of the experiments. In order to standardize these, different stages have been identified, and definitions of certain terms have been suggested, for use in the future. The methods of calculating different properties, as well as weight and volume of discharged sediment are described in the paper for use in other applications concerning deep-sea discharges.