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1.
高效液相色谱法测定海水中溶解态游离氨基酸 总被引：1，自引：0，他引：1
采用邻苯二甲醛柱前衍生-高效液相色谱-荧光检测器(OPA—HPLC-FLD)联用技术分离测定了海水中的14种主要溶解游离氨基酸(DFAA),通过邻苯二甲醛—3-巯基丙酸(OPA—3-MPA)柱前衍生后,在XDB-C18柱上分离。不同氨基酸测定的精密度(RSD)为1.62%~3.80%,检测限为11.4~69.7 ng.L-1,海水加标回收率在92%~110%之间。利用该方法测得青岛近海表层海水中氨基酸浓度为0.015~0.284μmolL-1。 相似文献
2.
柱前衍生-RP-HPLC方法测定水产品中生物胺 总被引：1，自引：0，他引：1
建立同时测定水产品中多种生物胺的丹磺酰氯柱前衍生反相高效液相色谱方法。用5%TCA提取样品中生物胺,正己烷脱脂,正丁醇/氯仿(1/1,v/v)萃取,以1,7二胺庚烷为内标,丹磺酰氯为衍生剂衍生后,采用CAPCELL PAK C18MG(4.6 mm I.D.×150 mm,5μm)色谱柱,以甲醇/水为流动相,进行梯度洗脱,流速1.5 mL/min。荧光检测器的激发波长(Ex)350 nm,发射波长(Em)520 nm。结果显示:色胺、苯乙胺、腐胺、尸胺、组胺、酪胺、精胺和亚精胺等8种生物胺在30 min内完全分离。在给定的浓度范围内,待测生物胺峰面积与内标峰面积之比同其相应浓度呈良好的线性相关(r>0.99)。仪器重复性良好(RSD<1.34%),方法重复性也在可接收范围内(RSD<10%)。除色胺(57.7%)外,其它7种生物胺的样品平均回收率均在94.2%~110.3%之间。结果表明生物胺的HPLC检测方法,分离度好,灵敏度高,可快捷、准确地对水产品中生物胺进行定性和定量检测。 相似文献
3.
本文建立了测定海力特胶囊含量和体外溶出度的高效液相色谱方法。采用 Aminex HPX-87H(30 0 mm× 7.8mm)柱 ,以 0 .0 0 2 5 mol· L-1H2 SO4 为流动相 ,柱温为 6 5℃ ,流速为 0 .5 m L·min-1,以示差检测器检测 ,外标法峰面积定量。本法测定线性范围为 1μg～ 4 0μg,方法平均回收率为96 .1% ,RSD为 0 .83% (n=5 ) ,体外溶出度测定结果为 96 %～ 99%。本法测定海力特胶囊含量和溶出度 ,具有方法简便、快捷 ,重复性好的特点 ,可作为制剂质量控制方法。 相似文献
4.
氟苯尼考在中国对虾体内消除规律的研究 总被引：2，自引：0，他引：2
采用口服药饵的方法研究氟苯尼考在中国对虾体内的代谢动力学和残留规律,用反相高效液相色谱测定氟苯尼考在对虾组织中的含量。结果表明:中国对虾连续5 d口服氟苯尼考药饵,高、低2种剂量(16 mg/kg.d和8 mg/kg.d)组的药物代谢动力学变化趋势相似,高剂量组的组织中药物含量远高于低剂量组,肝脏中的药物浓度远大于肌肉中的药物浓度,氟苯尼考在对虾体内的消除速度较快,低剂量组的消除速度比高剂量组快,2种剂量的药物在对虾肌肉中的消除曲线方程分别为C(t)高=0.247 3 e-0.015 5 t和C(t)低=0.118 2 e-0.043 2 t,消除半衰期分别为44.71 h和16.04 h。在本试验条件下,高、低2种剂量的氟苯尼考在肌肉组织中降到0.01,0.05,和0.1μg/g不同浓度水平的理论时间为:207,103,58,57,20和4 h。 相似文献
5.
应用分步电泳法检测水溶液和大鼠尿液中的古糖酯 (Propyleneglucol Guluronate SodiumSulfate,PGSS) .该醋酸纤维膜电泳选用两种电泳液 :(1) 0 .1mol· L-1的醋酸锌溶液 ,p H6 .0 ;(2 )1.0 mol· L-1的醋酸钡溶液 ,p H5.0。电泳膜于 0 .5%阿利辛兰水溶液中染色 ,1%醋酸溶液褪色。该法能够检测不同介质中的古糖酯 ,水溶液中的检测下限为电泳膜上加样 10 0 ng,尿液中古糖酯浓度高于 50 0 ng/ m L,经提取可以用此法测得。实验证实该法灵敏、稳定性高、重现性好。 相似文献
6.
以 6 -氨基喹啉 - N-羟基琥珀酰亚胺基氨基甲酸酯 (AQC)为衍生剂 ,与毛蚶抗贫血口服液中的氨基酸柱前定量衍生 ,用 Waters HPL C仪 ,Acc Q- Tag TM专用 C18柱 (3.9mm× 15 cm) ,以140 mmol· L-1的醋酸钠溶液 (p H5 .0 2 )为溶剂 A,乙腈为溶剂 B,超纯水 (Milli- Q水 )为溶剂 C,进行梯度洗脱 ,检测波长为 2 4 8nm,35 min测试完毕。各种氨基酸测定的重现性 RSD%均 <3.0 %(n=5 )。该方法简便快速 ,结果准确可信。 相似文献
7.
建立检测鸡鸭血浆中喹烯酮的方法,并测定其与鸡鸭血浆蛋白的结合率。采用平衡透析法测定喹烯酮的血浆蛋白结合率;血浆样品采用乙腈沉淀蛋白后用HPLC测定喹烯酮含量,同时采用HPLC测定透析外液中喹烯酮的含量,计算喹烯酮的血浆蛋白结合率,并对检测方法的方法学进行验证。建立的测定鸡鸭血浆中喹烯酮的方法,喹烯酮添加浓度为0.3、1和2μg/mL时,回收率范围为86.5%~92.2%,相对标准偏差均低于5%。喹烯酮在不同浓度的鸡鸭血浆中的平均蛋白结合率分别为40.53%±1.09%和46.88%±1.25%。喹烯酮药物浓度在0.5~8μg/mL的浓度范围内其血浆蛋白结合率无显著差异,其蛋白结合呈现非浓度依赖性。上述结果表明,喹烯酮在鸡鸭中应用时不易发生血浆蛋白结合介导的药物相互作用,药物的安全性较高。 相似文献
8.
目的：采用双波长HPLC同时测定参橘草营养强化饮液中5种化合物(腺苷、虫草素、人参皂苷Rg1、人参皂苷Re、橙皮苷)的含量。方法:依利特Hypersil BDS C18色谱柱(4.6 mm×250 mm,5 μm);流动相：乙腈-水,梯度洗脱;流速：1.0 ml/min;柱温25℃;检测波长203 nm(人参皂苷Rg1、人参皂苷Re),260 nm(腺苷、虫草素、橙皮苷)。结果：5种化合物在各自的浓度范围内均呈现良好的线性关系(r>0.9990),平均加样回收率（n=6）分别为96.72%、97.93%、98.04%、99.22%、101.69%。结论：该法简单快捷、稳定可靠,准确率高,重复性好,可用于参橘草营养强化饮液的质量评价。 相似文献
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以海带岩藻聚糖硫酸酯粗多糖为原料,采用Cu2+-H2O2自由基氧化体系结合超滤技术制备低分子量岩藻聚糖硫酸酯.通过比较粗糖质量和H2O2浓度对产物的分子量和化学组成的影响,确定制备高硫酸根高岩藻糖的低分子量岩藻聚糖硫酸酯的最佳条件是:4.5％ H2O2与0.026 7 mol/L Cu2+降解4.5g岩藻聚糖硫酸酯,得到Fa3(Mw7.68kDa)和Fb3(Mw 3.89kDa)2个组分,其硫酸根含量较高,为30.32％和32.48％.Fa3组分主要由岩藻糖(64.25％)和半乳糖(30.74％)组成,而Fb3的硫酸根和半乳糖含量高于Fa3,但岩藻糖含量下降.比较发现,H2O2浓度由4.5％上升为9％时,制备的低分子量岩藻聚糖硫酸酯的分子量、岩藻糖含量和硫酸根含量都下降.研究发现Fa3和Fb3对流感病毒神经氨酸酶具有较强的抑制作用,尤其是Fa3组分活性较高.说明分子量对岩藻聚糖硫酸酯的神经氨酸酶抑制活性影响要大于硫酸根含量,而且Fa3组分对流感病毒神经氨酸酶的抑制活性也可能与其单糖组成较均一有关. 相似文献
10.
目的：观察关节软坚止痛片对兔膝骨关节炎（KOA）模型血清及关节液中白细胞介素-6（IL-6）、肿瘤坏死因子-α（TNF-α）的影响。方法：将40只新西兰兔随机分为5组：空白组、模型组、玻璃酸钠组（对照组）及关节软坚止痛片低、高剂量组（简称为低、高剂量组）,每组各8只。采用屈曲位石膏铁丝固定法建立兔KOA模型后进行药物干预。观察比较各组肉眼下股骨内外髁组织,血清及关节液中IL-6、TNF-α含量,光镜下软骨组织形态学及Mankin''s评分。结果：各组血清及关节液中IL-6、TNF-α水平及Mankin''s评分比较,模型组均高于空白组、对照组及低、高剂量组（P<0.05）,对照组均高于低、高剂量组（P<0.05）,低、高剂量组比较,差异无统计学意义（P>0.05）。肉眼下股骨内外髁组织观察及光镜下软骨组织形态学观察结果显示：对照组及高、低剂量组均优于模型组,高、低剂量组均优于对照组。结论：关节软坚止痛片可治疗兔膝骨关节炎,其疗效优于玻璃酸钠注射液治疗,其作用机制可能与抑制IL-6、TNF-α等炎性因子表达有关。 相似文献
11.
Chandralata Raghukumar G. Sheelu P. A. Loka Bharathi Shanta Nair C. Mohandass 《Marine Georesources & Geotechnology》2001,19(1):1-16
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. 相似文献
12.
Arne Schnack-Friedrichsen Angela M. Davis Jim D. Bennell Dei G. Huws 《Marine Georesources & Geotechnology》2001,19(4):221-243
The interdependence between the seismo-acoustic properties of a marine sediment and its geotechnical/physical parameters has been known for many years, and it has been postulated that this should allow the extraction of geotechnical information from seismic data. Though in the literature many correlations have been published for the surficial layer, there is a lack of information for greater sediment depths. In this article, a desktop study on a synthetic seafloor model illustrates how the application of published near-surface prediction equations to subsurface sediments (up to several tens of meters burial depth) can lead to spurious predictions. To test this further, acoustic and geotechnical properties were measured on a number of sediment core samples, some of which were subjected to loading in acoustically-equipped consolidation cells (oedometers) to simulate greater burial depth conditions. For low effective pressures (representing small burial depths extending to around 10 meters subsurface), the general applicability of established relationships was confirmed: the prediction of porosity, bulk density, and mean grain size from acoustic velocity and impedance appears generally possible for the investigated sedimentary environments. As effective pressure increases through, the observed relationships deviate more and more from the established ones for the near-surface area. For the samples tested in this study, in some instances increasing pressure even resulted in decreasing velocities. There are several possible explanations for this abnormal behavior, including the presence of gas, overconsolidation, or bimodal grain size distribution. The results indicate that an appropriate depth correction must be introduced into the published prediction equations in order to obtain reliable estimates of physical sediment properties for greater subsurface depths. 相似文献
13.
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。 相似文献
14.
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. 相似文献
15.
Shigehisa Nakamura 《Marine Geodesy》2000,23(1):55-61
Specific properties of the interannual sea level variations and annual tides in the Northwestern Pacific were studied. Several tide stations were monitored. The monthly mean sea level for the year of 1995 was analyzed at each tide station. A seismic event in 1995, some tectonic activity around the subject area, and the Kuroshio (the oceanic western boundary current) may possibly contaminate results which would have occurred from the astronomical annual tide alone. 相似文献
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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. 相似文献
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Phylogenetic diversity and phenotypic characterization of cultivable bacterioplankton isolated from polar oceans 总被引：1，自引：0，他引：1
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. 相似文献
20.
The effect of different fixation and storage protocols on the flow cytometric (FCM) simultaneous analysis of bacterioplankton and phytoplankton in coastal seawater samples (Mediterranean coastal lagoons) was investigated. FCM measurements (cell number, fluorescence and scatter characteristics) were obtained through DAPI staining. Three fixatives [glutaraldehyde (GA), formaldehyde (FA) and paraformaldehyde (PFA)] and two storage (3 months duration) methods (5 °C and −196 °C) were tested. Two dominant populations were detected in studied samples: bacteria and eukaryotic picophytoplankton. Adding fixatives (2% final concentration) appears necessary to obtain FCM exhaustive counts of all the bacteria and phytoplanktonic cells. This was related to the permeation effect of fixatives which allowed a better DAPI staining of the cells. Maximum fluorescence, i.e. optimal staining of the cells was obtained with FA or PFA, and significant lower fluorescences with GA. Fixed samples stored at 5 °C induced rapid cell loss. Only storage in liquid nitrogen of samples fixed with FA or PFA, allows mid-term (≥4 months) preservation of bacteria or picophytoplankton cell numbers, and limited evolution of DAPI-induced fluorescence and scatter characteristics. 相似文献