跨海集群工程节能减排关键技术研究

港珠澳大桥跨海集群工程囊括跨海桥梁、沉管隧道、离岸人工岛等多个领域。跨海集群工程由于建设期及运营期能耗巨大,国内外尚无节能减排的成套技术指导工程建设,成为制约跨海集群工程持续发展的瓶颈之一。本文依托港珠澳大桥跨海集群工程建设和运营过程,采用理论研究、数值分析及模拟测试等多种方法,开展了集群工程节能减排指标体系和长大沉管隧道通风、照明、人工岛运营节能减排关键技术研究,成果支撑了工程项目节能减排目标的实现

Preparative Separation of Salvianolic Acid B from Salvia miltiorrhiza by High Speed Counter-Current Chromatorgraphy

采用高速逆流色谱法分离纯化丹参水溶性成分丹酚酸类物质,制备丹酚酸B化学对照品。分离采用的溶剂系统为正己烷-乙酸乙酯-水-甲醇(1.5:5:5:1.5),上相做固定相,下相做流动相,流速为1.7 mL/min,仪器转速850 rpm,进样量80 mg,纯度用HPLC方法测定。结果表明:一次分离可制备63.4 mg丹酚酸B,其纯度为98.6%。该方法操作简单,可作为高纯度丹酚酸B化学对照品的制备分离方法。Salvianolic acid B,a major bioactive component in Danshen(Salvia miltiorrhiza Bge.),was isolated and purified by high-speed counter-current chromatography(HSCCC) in semi-preparative scale from the crude extract of Danshen.Separation was performed with a two-phase solvent system composed of hexane-ethyl acetate-water-methanol(1.5:5:5:1.5,v/v) by eluting the lower aqueous phase at a flow-rate of 1.7 mL/min and a revolution speed of 850 rpm with injection volume of 80 mg.After the proceeding of separation,63.4 mg salvianolic acid B was obtained,and analyzed by normalization method according to HPLC areas giving a purity of 98.6%.HSCCC is a recommendable method to prepare and purify the active constituents from Salvia miltiorrhiza.国家自然科学基金重点项目(20235020);; 厦门市科技创新重点项目(3502Z20031096

Study on the Preparation of Salvianolic Acid B of High Purity

目的:建立高纯度丹酚酸B的最佳制备工艺流程。方法:通过比较几种不同大孔吸附树脂对丹酚酸B的吸附及洗脱性能,筛选出最佳树脂并对该树脂分离纯化丹酚酸B的工艺参数进行优化。结果:在本文所确定的最佳工艺条件下,丹酚酸B回收率为90.6%,纯度高达91.8%,稳定性良好,可作为丹参制剂的原料药应用。结论:该工艺操作简便,适用于工业化生产,有利于促进丹酚酸B的开发利用。Objective:The best technology of the preparation of salvianolic acid B was established.Methods:A series of macroporous adsorption resins were compared on their adsorption and desorption properties for salvianolic acid B and the optimal type resin had been selected. The technical parameters for purification of salvianolic acid B with the selected type resin were studied. Results:Under this condition, the recovery is 90.6% and the purity of salvianolic acid B is 91.8%. The product has a good stability and could be used for preparation directly.Conclusion:This method is simple and could be used for industrial production, promoting the exploitation and utilization of salvianolic acid B.国家自然科学基金重点项目(No.20235020);; 青岛市重点实验室建设项目(No.04-2-JS-135

Methodologic Study of HPCE Fingerprints of Radix paeoniae Alba and Radix paeoniae Rubra

目的确定赤芍和白芍的高效毛细管电泳分析方法,建立赤芍和白芍的高效毛细管电泳法(HPCE)指纹图谱。方法HPCE工作条件:采用未涂层熔融石英毛细管(内径75μm,有效长度50 cm),分离电压为25 kV,柱温25℃,二极管阵列检测器(DAD)检测波长为220 nm,缓冲液为30 mmol/L硼砂(pH=9.0)溶液。按此条件对来自不同产地的7种赤芍样品和8种白芍样品进行了分析。结果建立了赤芍和白芍HPCE指纹图谱,采用中药指纹图谱相似度计算软件,以系统生成的对照指纹图谱为对照模板对不同样品的图谱进行相似度计算。结论该方法简捷、有效,可以用于赤芍和白芍药材的质量控制。Objective To set up a modern High Performance Capillary Electrophoresis analysis method for separating and detecting Radix paeoniae Alba and Radix paeoniae Rubra and establish their fingerprints.Methods Seven samples of Radix paeoniae Alba and eight samples of Radix paeoniae Rubra were carried out by HPCE under the following conditions: bared fused silica capillary(50 cm ×75 μm i.d.),30 mmol/L borate(pH = 9.0) as buffer,the run voltage is +25 kV,detection wavelength of UV at 220 nm,and column temperature of 25℃.Results The fingerprints were confirmed and compared by the software of the similarity evaluation system for chromatographic fingerprint.Conclusion The results showed that the method of HPCE fingerprint is reliable and accurate to control the quality of two Chinese traditional medicines.国家自然科学基金重点项目(No.20235020);; 青岛“2004将才计划”(No.04-3-JJ-11);; 青岛市崂山区科技计划项目(No.LS-05-KJZX-76

Determination of Pseudostellarin B in Pseudostellaria heterophylla by HPCE and Study on Its Fingerprints Analysis

建立了测定太子参中环肽Pseudostellarin B含量的高效毛细管电泳(HPCE)分析方法,对10种不同产地太子参中环肽Pseudostellarin B的含量进行了测定。HPCE工作条件:采用未涂层熔融石英毛细管(内径75μm,有效长度50cm),分离电压为15kV,柱温20℃,二极管阵列检测器(DAD)检测波长为203nm,缓冲液为20mmol/L硼砂(pH=9.3)溶液。在选定的工作条件下,环肽Pseudostellarin B浓度与其响应信号值之间具有较好的线性相关性(Y=0.6357X+2.546,R=0.9985),加标回收率在93.8%~105.6%之间。在此基础上进行了太子参HPCE指纹图谱研究,采用中药指纹图谱相似度计算软件对不同太子参样品的HPCE指纹图谱进行相似度计算,以系统生成的对照指纹图谱为对照模板,10份样品中有8份的相似度在0.90以上,说明该方法可用于太子参质量控制。A modern HPCE analysis method was developed for determinating cyclic peptide Pseudostellarin B in Pseudostellaria heterophylla(Miq.) Pax.Separation and determination were carried out by HPCE under the following conditions: bared fused silica capillary (50 cm×75 μm i.d.),20 mmol/L borate (pH=9.3)as buffer,the run voltage is +15 kV,detection length of UV at 203 nm,and column temperature of 20 ℃.The results indicated that the developed method was simple,accurate and reliable for the determination of Pseudostellarin B with a good linearity(Y=0.6357X+2.546,R=0.9985),and the recovery ranges of 93.8%～105.6%.Based on this method,the HPCE fingerprints of Pseudostellaria heterophylla (Miq.) Pax were established.The fingerprints were compared by the software of the similarity evaluation system for chromatographic fingerprint.The fingerprint congruence coefficients of 8 electropherograms in 10 were above 0.90.The method of HPCE fingerprint is reliable and accurate.国家自然科学基金项目(20235020);; 国家科技部攻关项目(2003BA759C

海洋现场叶绿素传感器的校准方法初探

采用单一藻种培养液校准海水现场叶绿素传感器,讨论了校准方法及传感器应用在海洋调查中的可行性,结果发现,利用威氏海链藻(Thalassiosira weissflogii)的培养液校准叶绿素传感器,叶绿素浓度与荧光信号线性关系良好,相关系数R2均大于0.995,每次实验的校准斜率误差均小于5%,表明利用藻液校准叶绿素传感器是可行的,具有可重复性。然后利用传感器与荧光分光光度法测量同一系列藻液,t检验法分析表明当叶绿素浓度大于5μg/L时,两种方法无显著差异;当浓度小于5μg/L时存在显著差异,传感器测量结果偏大;可能是高温、光照等影响荧光分光光度法测量结果。就荧光分光光度法而言,叶绿素传感器可以比较准确地评价水体的叶绿素浓度,不仅可以为浮游植物动力学提供依据,还可以为赤潮预警等提供数据支撑

InGaAs/GaAs应变量子阱的低温光伏谱

用光伏谱方法研究了IngAAS/gAAS应变量子阱结构中各子能级间的光跃迁，并与理论计算的结果进行了比较.分析了光伏谱峰能量随阱宽与温度的变化，并讨论了光伏谱峰强度的温度关系.国家自然科学资金;福建省自然科学基

Classification of Panax Quinquefolium.L Samples by Cluster Analysis

建立西洋参药材分类方法;分别采用电感耦合等离子体质谱(ICP-MS)法、高效液相色谱(HPLC)法以及蒽酮-硫酸分光光度法,对12个西洋参样品中的15种无机元素、7种人参皂苷和多糖进行测定,用SPSS聚类分析法对12个西洋参样品进行聚类分析;结果表明:以4种不同的聚类变量进行聚类分析,其聚类分组结果并不一致,将几种有效成分综合为聚类变量,对西洋参进行分类更为科学合理;聚类分析法是西洋参分类分析的有效方法,对西洋参品种与质量的鉴定有一定的理论意义和实用价值。A classification method was developed for the quality assessment of Panax Quinquefolium.L.The contents of fifteen elements,seven ginsenosides and polysaccharide in twelve Panax Quinquefolium.L samples were determined by ICP-MS,HPLC and anthrone-sulfuric acid spectrophotometry,respectively.The cluster analysis was applied for the classification of 12 Panax Quinquefolium.L samples.The analysis results showed that the classified results were different with different cluster variables and it was found more reasonable to integrate several active components as cluster variables for the classification.The cluster analysis was useful for the classification of Panax Quinquefolium.L

Determination of Theanine in Tea by High Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Mass Spectrometry

采用高效液相色谱-大气压化学电离质谱(HPlC-APCI-MS)联用技术,建立了茶叶中茶氨酸的含量测定方法。实验采用C8柱,以甲醇-水为流动相,等度洗脱,采用正离子大气压化学电离质谱(SIM模式)进行测定,可以获得稳定的质谱信号,并采用正交实验设计对APCI-MS仪器条件进行了优化。结果表明,本文建立的HPlC-APCI-MS方法操作简便、重现性好,灵敏度较紫外检测器有很大的提高,可用于微量茶氨酸的快速测定。HPLC coupled online with atmospheric pressure chemical ionization MS technique was developed for the qualitative and quantitative determination of theanine in tea.The theanine and other compounds in the tea extract were separated on an Alltima C8 column with methanol and water (10:90 v/v) as mobile phase, with flow rate of 0.6 ml/min and APCI-MS SIM m/z 175.1 detection.In the positive APCI mode, sensitive and stable MS signal could be obtained by APCI-MS (SIM m/z 175.1) detection, and the APCI-MS conditions were also optimized by orthogonal design.The results indicated that HPLC-APCI-MS method was simple, sensitive and reliable for the determination of theanine in tea.It was important that the detection sensitivity was improved greatly by APCI-MS than UV.Eight tea samples from Fujian province were analysed using the established methods.福建省科技厅茶叶指纹图谱质量控制研究项目(2006N0043);海洋一所基本科研业务专项(GY-022008T32)资

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