Concentration and distribution of polycyclic aromatic hydrocarbons in surface sediments collected in the Southern Yellow Sea

采用气相色谱与质谱联用(gC/MS)技术,在一个航次内对南黄海表层沉积物中16种优先监控的PAHS的污染状况进行了调查,采用菲/蒽、荧蒽/芘、荧蒽/(荧蒽+芘)、吲哚芘/(吲哚芘+苯并(g,H,I)苝)等特定比值对PAHS来源进行了分析.结果表明,南黄海表层沉积物中检出PAHS的总含量为90.4~732.65ng·g-1,各站点均以4~6环为主;与其它站位相比,倾废区的H01站位受到PAHS污染较为明显,无论是16种PAHS总量还是高分子量组分最高值都出现在该站点,虽然该海区沉积物中PAHS的含量没有超出生物影响低值,但苯并(b)荧蒽、吲哚芘和苯并(g,H,I)芘等一些没有最低安全标准的PAHS也有不同程度的检出,对海洋生物具有潜在的毒副作用.PAHS可能来源于原油、生物和煤燃烧造成的污染.The concentrations of sixteen representative Polycyclic Aromatic Hydrocarbons(PAHs) in surface sediment samples collected from the Southern Yellow Sea were determined by GC-MS.The distribution and potential sources of PAH contamination in the region were investigated.The types of PAHs found in the surface sediments were mainly 4～6 ring PAHs,and they are unevenly distributed among the different sampling sites covering an area of 139 km2.The area is known for continuous waste dumping activities in recent years,and indeed sites adjacent to such activities were found to have high levels of PAHs.Some high molecular weight PAH compounds such as benzo$$b$$fluoranthene,dibenzo$$a,h$$anthracene and benzo$$g,h,i$$perylene were detected in some samples.The health implication of these contaminants needs careful assessment since toxicity guidelines are not available for these species.The potential sources of PAHs are discussed using various source-specific PAH indexes such as Phenathrene/Anthracene、Fluoranthene/Pyrene、Fluoranthene/(Fluoranthene+Pyrene) and Indeno [1,2,3-cd] pyrene/(Indeno[1,2,3-cd] pyrene+Benzo [g,h,i] perylene).The composition of the observed PAHs reflects that they originate from both petroleum utilization and incomplete combustion.海洋公益性行业科研专项(No.200705011);中国海监技术支撑体系项目;2008年海洋环境保护及节能减排专项---

Comparison of Recoveries of PAHs Obtained by Ultrasound-assisted Extraction from Wet and Freeze-dried Marine Sediment

以美国环保局(EPA)优先控制的16种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)为研究对象,建立了湿法超声波辅助萃取技术提取沉积物中痕量PAHs的可靠方法,对萃取剂、萃取功率、萃取次数和萃取时间进行了优化。并与传统干法超声辅助萃取进行了比较,湿法超声波辅助萃取的PAHs回收率为57%～125%,而干法超声波辅助萃取PAHs的回收率为48%～113%,对相对分子质量小的PAHs如萘～芴的回收率,湿法明显高于干法。该文建立的湿法超声辅助萃取适用于沉积物和泥土中痕量PAHs的快速测定。An ultrasound-assisted extraction method for the extraction of 16 trace PAHs(USEPA priority pollutant) from wet(i.e.untreated) marine sediment was developed.The effects of solvent type,power of ultrasound,and extraction time were studied and optimized.The developed method was compared with the traditional ultrasound-assisted extraction for freeze-dried sediment.The results showed that recoveries of sixteen PAHs extracted from the wet marine sediment ranged from 57% to 125%,whereas those extracted from the freeze-dried marine sediment ranged from 48% to 113%.The results also indicated that the recoveries of PAHs with smaller relative molecular mass(e.g.naphthalene and fluorine) extracted from the wet sediment were higher than those from the freeze-dried sediment.Thus the developed method was appropriate for rapid determination of trace PAHs in marine sediment and soil.海洋公益性行业科研专项(200705011);; 中国海监技术支撑体系项目;; 2008年海洋环境保护及节能减排专

Evaluation of DPPH Free Radical Scavenging Capability of Hippocampus japonicus Kaup. and Their HPLC Fingerprint

目的采用体外1,1-二苯基苦基苯肼(dPPH)抗氧化模型对海马提取物的抗氧化性质进行评价,并建立小海马HPlC特征指纹图谱,用于小海马药材的鉴别及质量评价。方法利用离线dPPH抗氧化评价体系对海马不同提取物进行评价,结果表明,海马水提物抗氧化能力最强,在此基础上又探明了海马水提物抗氧化能力随时间和浓度的变化规律,为海马抗氧化活性提供了科学依据。依据抗氧化活性实验结果,建立了海马水提物HPlC特征指纹图谱分析方法。结果海马水提物大部分化合物达到基线分离,方法的精密度、重现性、稳定性良好;建立小海马药材HPlC指纹图谱,采用中药指纹图谱相似度计算软件,对小海马进行真伪辨别和质量评价。结论表明该方法简捷、有效,是小海马药材鉴别及质量控制的有效方法。OBJECTIVE To evaluate the antioxidant activity of the extracts of Haima,and to establish the HPLC fingerprint of Haima for the discrimination and the quality evaluation of Haima.METHODS Antioxidant properties of Haima extracts with different solvent were assayed in terms of antioxidant activity by scavenging activities on 1,1-diphenyl-2-picrylhdrazyl(DPPH).The effect of time and concentration of Haima extract on the antioxidant activity was also studied.Secondly,a chromatographic fingerprint method was developed.RESULTS The antioxidant activity of water extract of Haima was higher than all the other extracts of Haima.The developed HPLC method was simple,accurate and reliable for the development of Haima fingerprint.Ten Haima samples collected from different medicine store were analyzed and the Haima HPLC fingerprint was established.The similarity of the HPLC chromatogram was performed for authentication and quality control of Haima.CONCLUSION The HPLC fingerprinting techniques have high potential in authentication or source-tracing types of applications.国家自然科学基金重点项目(20235020);青岛市共建生物医药研发测试中心资助项目(LS-05-KJZX-76

Identification of Bohai Sea crude oil based on characteristic fingerprinting by MSPD-RP-HPLC

建立渤海原油的高效液相色谱(HPlC)特征指纹图谱,为渤海原油的鉴别提供一种新方法。以氧化铝作为基质固相分散剂进行样品处理,采用HPlC法进行分析,双反相C18色谱柱串联,以乙腈-水为流动相,二元线性梯度洗脱,流速为1.0 Ml/MIn,柱温为20℃,双波长检测226 nM、254 nM,进样量10μl;采用所发展的方法对10批渤海原油样品进行分析,建立渤海原油的HPlC特征指纹图谱,结合相似度分析用于渤海原油的鉴别。该方法具有很好的精密度、重复性和稳定性,10批渤海原油特征指纹图谱有13个共有峰,结合相似度分析可以用于渤海原油样品的鉴别,说明HPlC特征指纹图谱是渤海原油鉴别的有力工具。Based on the high performance liquid chromatography(HPLC) characteristic fingerprinting,a new method for crude oil identification of Bohai Sea was developed.The sample pretreatment was done using matrix solid-phase dispersion,and Al2O3 was used as the dispersant.The chromatographic fingerprints were determined by injecting 10 L sample solution each time on two reverse phase C18 columns in series with the gradient elution solvent system composed of water and acetonitrile.The flow rate was 1.0 mL/min,the column temperature was maintained at 20℃ and the signals were acquired at 226 nm and 254 nm.The characteristic fingerprints of crude oil were established by analysis of ten representative samples derived from Bohai Sea,and identification was carried out by the similarity analysis of the characteristic fingerprints.The method was ideally suited for the fingerprinting of Bohai Sea crude oil with good precision,repeatability and stability.13 peaks were selected as the common peaks of the characteristic fingerprint and used for the similarity analysis,which could be applied to distinguish crude oil of Bohai Sea from that of other sources.The characteristic HPLC fingerprinting technique thus was a powerful tool for the identification of crude oil originated from Bohai Sea.海洋公益性行业科研专项(200705011;201005034-3);中国海监技术支撑体系项目;2008年海洋环境保护及节能减排专

基于有限元法的新型双脊波导传输特性的研究

文章采用有限元法研究了圆形和椭圆形两种变形对称双脊波导对传输特性的影响。计算了脊的尺寸变化时的截止波长和单模带宽,给出了主模场结构图以及变形对截止波长和单模带宽影响的关系曲线,并分析了传输特性随对称脊波导结构尺寸变化的情况。通过这些研究,能够为变形双脊波导的应用和研究提供有价值的参考

小管道离散泡状流的形成与发展

航天(尤其是大型载人航天及深空探测)技术的发展,激发了对微重力气液两相流研究的强烈需求和兴趣。在航天应用中小直径

山东半岛北岸不同生境潮间带浮游细菌多样性研究

通过提取山东半岛北岸不同类型潮间带海水样品的总DNA,构建16S r DNA文库,利用群落相似性分析(ANOSIM)和非度量多维尺度转换排序(NMDS),探究潮间带类型对浮游细菌群落结构的影响,并对比了与近海浮游细菌群落结构的差异。分析结果显示,浮游细菌的丰度及多样性受到潮间带类型的影响,烟台养马岛泥滩、石滩、辛安河沙滩、黄河三角洲碱蓬区和天鹅湖海草区以变形菌门占优势,而黄河三角洲米草区以拟杆菌门为优势菌,其中,天鹅湖海草区浮游细菌的丰富度和多样性最高。潮间带海水中浮游细菌的组成与近海存在显著差异,潮间带浮游细菌的丰度及多样性均显著高于近海。推测季节因素、植被类型、有机质来源可能是造成潮间带不..

Applications of HPLC-MS in the Rapid Identification of Components in Marine Medicinal Organisms

高效液相色谱-质谱联用(HPlC-MS)技术,将HPlC的高分离效能与MS的强大结构鉴定功能结合起来,已逐渐成为天然产物化学成分快速分离、鉴别的强有力手段。本研究采用高效液相色谱-电喷雾质谱联用(HPlC-ESI-MS)技术,成功建立了刺参皂苷快速鉴别方法,并对市售干刺参中的4种皂苷进行了鉴别。此外,应用该技术对罗氏海盘车中的13种化学成分进行了快速鉴别。为海洋药用生物化学成分快速鉴别提供了1种值得推广的新方法,为更好的开发利用海洋天然药物奠定了基础。In recent years,high performance liquid chromatography-mass spectrometry combined the high separation efficiency of HPLC with rapid identification function of MS had become a powerful tool for the rapid separation and identification of chemical components in natural products.In the present study,a high performance liquid chromatography-electrospray ionization mass spectrometry(HPLC-ESI-MS) method was developed for rapid identification of 4 saponin components in dry Holothurian sold on the market.On the other hand,13 compounds in Asterias rollestoni were also identified by HPLC-ESI-MS.The HPLC-MS method presented in this paper for the rapid identification of marine compounds was worth popularizing and to lay a foundation for the further exploration of marine natural products.国家自然科学基金项目(20675021;20905017);中国近海海洋综合调查与评价908专项项目(908-02-05-04);海洋局青年基金资