晕清降压胶囊的质量标准研究

目的：建立晕清降压胶囊薄层色谱鉴别方法和高效液相色谱含量测定方法,制定其质量标准。方法：薄层色谱鉴别山楂、天麻,液相色谱测定天麻素和黄芪甲苷含量。结果：薄层色谱鉴别色谱中,供试品色谱在与对照药材色谱和对照品色谱相应的位置上,显相同颜色的斑点,阴性样品无干扰。天麻素在0.0505～0.404μg范围内具有良好的线性关系,黄芪甲苷对照品在2.56～7.68μg范围内线性关系良好。结论：该方法操作简便、准确可靠、重复性好,可为制定晕清降压胶囊的质量控制标准提供参考依据。     

一种检测溢油的快速分类辅助鉴别方法

用气相色谱法和气相色谱-质谱法分析了原油样品的正构烷烃和甾萜烷生物标志物。针对在仪器分析过程中由各种因素带来的采集点漂移的现象,利用相关系数校正方法对保留时间进行了校正。实验结果表明,保留时间校正后大大提高了采集点的重合性。采用欧氏距离方法对校正后的色谱数据进行聚类分析,基于色谱数据的聚类分析对于降解油和非降解油的分类效果良好;而基于校正后甾、萜烷生物标志物数据的聚类分析结果能很好的将溢油样品与溢油源样品聚为一类,而与其他不相干油田的样品区分开来,聚类分析结果更能真实反映样品的真实信息。相关系数校正与快速聚类分析方法相结合为溢油来源的判断提供了一种快速分类辅助鉴别方法。     

海洋细菌脂肪酸的气相色谱分析

以副溶血性弧菌VP-X-3为试验对象,利用气相色谱技术分析了其细胞脂肪酸的组成和含量,以色谱峰的数量、色谱峰高及脂肪酸含量作为评价指标,探讨了不同的皂化和甲酯化条件对细菌细胞脂肪酸测定结果的影响。结果表明:皂化和甲酯化条件都对细胞脂肪酸的组成和含量产生一定的影响。较低温度皂化处理利于增加色谱峰数量和色谱峰高。甲酯化温度过高容易破坏脂肪酸,尤其是长链脂肪酸和不饱和脂肪酸的结构。高温甲酯化条件下,时间越长,甲酯化效果越差。试验得到较为理想的气相色谱前处理条件:2 mol/L NaOH-甲醇溶液2 mL,70℃水浴10 min;10%(V/V)H2SO4-甲醇溶液2 mL,70℃水浴15 min。此条件下的色谱峰的数量多达29种,色谱峰高明显高于其他处理条件下的峰高。     

海洋溢油鉴别前处理技术比较研究

针对目前海洋溢油样品的吸附色谱柱预分离前处理技术,比较了不同前处理方法得到的溢油样品中烃类化合物、生物标志物、金刚烷类化合物和多环芳烃类化合物的气相色谱／气相色谱质谱指纹图谱。就溢油样品吸附色谱柱预分离技术的优缺点进行了详细总结和讨论,并为溢油来源的快速、准确鉴别提出了建议。     

多环芳烃的海洋环境行为及其代谢产物的研究进展

多环芳烃是一类广泛存在于环境中的持久性有机污染物,具有"三致"作用.环境中多环芳烃的某些不完全代谢产物同样可能具有持久性,有些甚至比母体多环芳烃的毒性更强,有可能对环境造成更大的危害.本文介绍了近年来国内外有关多环芳烃的海洋环境行为及其代谢产物毒性方面的研究进展,并重点对代谢产物的分析方法,包括高效液相色谱、气相色谱、气相色谱-质谱联用和液相色谱-质谱联用等,进行了总结,最后对该领域的研究方向进行了展望.     

雌激素对水生生物的影响及其检测方法研究进展

综述了雌激素对水环境的污染现状及其对水生生物的影响,介绍了目前雌激素的检测方法,详细阐述了气相色谱和液相色谱及其联用技术在雌激素测定方面的最新研究进展,并对雌激素的研究方向进行了展望。     

HPLC色素分析技术在海洋浮游植物群落结构研究中的应用

高效液相色谱技术(High Performance Liquid Chromatography,HPLC)是一项成熟的分离分析技术。本文综述了基于HPLC的色素分析技术在浮游植物群落结构研究中的应用历程。对这一技术在野外采样、样品预处理、色谱信息获得以及数据处理等环节的要求进行了详细描述,并结合相关研究进行了HPLC方法与其他方法的对比。介绍并讨论了此项技术面临的问题、最新进展及今后的发展趋势。     

西沙海绵Plakortis simplex中的三个聚酮类成分研究

为了对海绵(Plakortis simplex)乙酸乙酯萃取物中的聚酮类化学成分进行研究,本文综合运用有机溶剂萃取、正相硅胶柱色谱、反相硅胶柱色谱(ODS)以及高效液相色谱(HPLC)等多种手段对海绵(Plakortis simplex)的弱极性化学成分进行分离纯化。通过MS和NMR波谱分析方法并结合文献对照,鉴定化合物的结构。从该海绵的乙酸乙酯萃取物中共分离鉴定了3个化合物。化合物2和3均为首次从该种海绵中分离得到。     

ICP-MS及其联用技术在海洋地质研究中的应用前景

电感耦合等离子体质谱(ICP—MS)具有灵敏度高、检出限低、选择性好、线性范围宽、能进行多元素和同位素比测定等优点,广泛应用于环境、地质、医药、食品和高纯物质等领域。ICP—MS与其他进样及分析技术的联用,大大地扩展了其应用范围。重点介绍了ICP—MS与激光烧蚀(LA)、高效液相色谱(HPLC)及气相色谱(GC)的联用技术,探讨了它们在海洋地质研究中的应用前景。     

天然气水合物气体组成分析技术

系统地分析了国内外有关天然气水合物气体组成分析技术的研究现状,对样品保存技术、气体分解与收集技术、仪器分析技术、数据处理技术以及模拟实验中的色谱在线分析技术分别进行了总结与评述,对开展天然气水合物气体组成分析方法研究提出了几点建议.     

Metallothionein induction by Cu, Cd and Hg in Dicentrarchus labrax liver: assessment by RP-HPLC with fluorescence detection and spectrophotometry

Metallothionein was quantified in sea bass Dicentrarchus labrax intraperitoneally (i.p.) injected with different Cu, Cd and Hg doses (50-250 microg kg(-1) wet wt) after 48 h exposure. A distinct peak with 16.8 min retention time was obtained by reversed-phase high performance liquid chromatography coupled to fluorescence detection (RP-HPLC-FD) with the three metals. Total metallothionein levels assayed in unheated liver extracts by RP-HPLC-FD were significantly higher (1.3-1.95-fold) than those obtained by the well-established spectrophotometric method. In the RP-HPLC-FD method, metallothionein increased linearly with Cu and Hg doses, being saturated beyond 100 mug kg(-1) Cd. Maximum induction was obtained at 100 microg kg(-1) Cd (5.3-fold), and 250 microg kg(-1) Cu or Hg (8- and 5.1-fold, respectively). At low doses no metallothionein induction was shown by the less sensitive spectrophotometric assay.     

泥蚶血红蛋白的制备及其抗菌活性研究

利用凝胶层析技术从泥蚶血细胞裂解物中分离纯化得到两种血红蛋白,回收率为74.3%,并通过Tricine-SDS-PAGE和质谱技术鉴定为Tg-HbⅠ(同源二聚体)和Tg-HbⅡ(异源四聚体)。分别通过琼脂扩散法和分光光度法测其抗菌活性和过氧化物酶活性,结果发现,两种Tg-Hb对大肠杆菌和恶臭假单胞杆菌均有抗菌活性,Tg-HbⅡ对于恶臭假单胞菌和大肠杆菌的MIC值分别为0.063mg/mL和0.13mg/mL,Tg-HbⅠ对两种菌的MIC均为0.048mg/mL;两种Tg-Hb均具有过氧化物酶活性,能催化愈创木酚、邻苯二酚、对苯二酚、苯酚、左旋多巴等多种酚类物质。在Tg-Hb中添加GSH后,两种Tg-Hb均不再对恶臭假单胞杆菌具有抗菌活性。可见,两种Tg-Hb对恶臭假单胞杆菌等的抗菌活性均是通过其过氧化物酶活性发挥作用的。     

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.     

Metal pollution assessment of the marine environment by determination of metal-binding proteins in Mytilus sp.

Adult mussels (Mytilus galloprovincialis) (shell length 5–7 cm) exposed to elevated concentrations of Cd (0.1–1.3 mg l⁻¹), in a flowing seawater aquarium under laboratory conditions, responded by elevated synthesis of metal-binding proteins in a digestive gland. Response depended on the Cd concentration level as well as on duration of the exposure time. Results obtained show that inducible proteins (isolated by gel-filtration column chromatography and characterized by electrochemical and spectrophotometric methods) should be considered metallothionein-like proteins.The induced metal-binding proteins of mussels in specific organs or tissues are considered to be a potential biological indicator of metal pollution, taking into account specific qualities of the mussel response to different metals. The advantages of the analytical methods applied (gel-chromatography and polarography) and the relevance of the laboratory data when transferred to environmental conditions are discussed. Previously reported results dealing with metal-binding proteins of Mytilus species are also summarized.     

Spectrophotometric and iodometric methods for the detection of hydrogen sulfide in the Black Sea: Comparison of the results of analysis

We discuss the results of analysis of published data and field and laboratory investigations aimed at the solution of the problem of comparabilityof the results of detection of hydrogen sulfide in the Black Sea by spectrophotometric and iodometric methods. We show that the reproducibility of the results of spectrophotometric analysis is higher than hat of the iodometric method only in the case where the content of sulfide in a sample is less than 10–30 μMl⁻¹. When larger concentrations are involved, the traditional iodometric analysis proves to be the most precise and reliable method for the detection of hydrogen sulfide in the Black-Sea waters. Translated by Peter V. Malyshev and Dmitry V. Malyshev     

海水中硼的测定方法

介绍了海水中硼的测定主要方法,包括容量法,分光光度法、极谱法、光谱法、离子选择电极法等及其研究进展。     

沉积物总氮总磷同时消解分析方法

对沉积物样品通过同时消解可分别测定总氮和总磷的方法作了探讨.总氮用次溴酸盐氧化比色法,比凯氏定氮法快速省时;总磷用钒钼酸铵比色法.采用同时消解沉积物样品,简化了分析操作流程,使分析条件与工作曲线酸度相同,因而取得较好的测定效果:总氮回收率102% ～105%,精密度3.6%;总磷精密度5.5%,测定值都在标准值范围之内,适用于批量测定.     

长江口嵊泗海域生物体内持久性污染物残留量及分布特征

利用2007年10月“908”项目调查期间采集于长江口嵊泗海域的生物样品,采用气相色谱和气相色谱质谱法对其有机氯农药和多氯联苯的含量和组分特征进行了定量分析,并结合其它河口地区资料进行了对比,探讨了其残留量和分布特征,结果表明:研究海域各生物体内HCHs的总量水平为(6.0～20.3)×10-9,平均值为12.13×1...     

离子交换剂直接比色测定海水中微量镉与铬

近年来,在一般分光光度法—比色法的基础上,发展起来了一个新方法,使得比色法似乎在返老还童,又可与原子吸收、放化分析、极谱法竞相争雄了。这个新方法就是离子交换剂直接比色法[1,2]这个方法的特点是(1)以半透明的离子交换剂为显色媒体直接进行光度测定;(2)离子交换剂能自稀溶液中富集待测成份,在一定条件下使待测成份在树脂上显色,之后不经过淋洗,即进行光度测定。这就把一般方法中“分离富集”和“光度测定”两步巧妙地合并成一步,结果使得本方法具有高灵敏度、简便快速等优点。但是,因为这一方法只是近年来才在文献上出现,所以在许多方面很不成熟,尚待不断改进和完善,特别是把此法应用到海水中微量元素的分析上,在文献上还未见有详细的和有效的研究结果报导。     

Liquid waveguide capillary cell for the spectrophotometric determination of nanomolar iodate concentrations in marine waters

A new spectrophotometric method based on a liquid waveguide capillary cell for an enhanced detection was developed to measure nanomolar iodate concentrations. This method has a detection limit and precision of 1–2 nmol/L, which is equivalent to 10% that of conventional methods, a recovery of 97.7%–104.0%, and a working range of 10–120 nmol/L. Water samples were collected from three estuaries and one coastal ocean for testing, and the proposed technique detected as low as 11 nmol/L and 18 nmol/L ...