关于从中国滇池微囊藻中分离出微晶体的初报

Isolates of Microcystis blooms collected from Dianchi Lake of South-western China in different seasons were tested by mouse bioassays. The LD₅₀ of the vcdcrocystis isolates corre-sponding M. wesenbergii, M.viridis and M. aeruginosa were 221 mg · kg ^-1, 188 mg · kg ^-1, and 198 mg · kg ^-1 respectively. The cells of the three samples contained hepatotoxins or microcystins. The HPLC (high performance liquid chromatography) analysis showed that all the three Microcystis species contained microcystin LR. In addition, M. wesenbergii contained microcystin RR, M. viridis contained microcystinYR, M. aeruginosa contained both microcystin RR and YR. The results suggested that in different seasons the toxins which were produced by the dominating Microcystis species were fluctuent with regard to the composition and content of the toxins and consen-quently were obvious factors that aroused the water quality to decrease and change.     

A high sensitivity, low volume HPLC method to determine soluble reactive phosphate in freshwater and saltwater

A reverse phase High Performance Liquid Chromatography (HPLC) method was developed to detect soluble reactive phosphate (SRP) in marine and freshwater samples. This technique is scalable over a range of sample volumes from 10 μl to 10 ml, requires minimal sample preparation, and responds linearly from 1 nM to 100 μM (R²>0.964). Standard Murphy–Riley molybdenum blue reagents were used to react with phosphate in samples for analysis. Solid phase extraction tubes were used to clean the mixed complexing reagent prior to combining the reagent with samples. The method was applied to freshwater samples collected in July 2001 along an Andean mountain stream located in the Eastern Cordillera (2400 m) of Peru and marine samples collected in January 2002 within the low marsh of the estuarine Nueces Delta System, Texas Coastal Bend. For method comparison, field samples were analyzed using a standard manual spectrophotometric method. Field sample phosphate concentrations produced from each method were nearly identical. This method offers the advantages of low sample volume (1 ml or less) with high sensitivity, precision, and potential automation.     

Spatial and temporal variations in free polyamine distributions in Uranouchi Inlet, Japan

Polyamines are an essential component of living organisms that influence normal cell growth and development. Despite the possible importance of polyamines for marine microbial ecology, concentrations of polyamines in seawater are not well known.Using HPLC analysis with a cation exchange column and OPA reagent, we determined polyamine concentrations in seawater without carrying out desalting, concentration or derivatization steps prior to chromatography.In seawater collected from Uranouchi Inlet, putrescine and spermidine were the predominant polyamines, ranging from undetectable (N.D.) to 4.4 nM and N.D. to 2.8 nM, respectively. Though other polyamines were detected, the frequency of detection was much lower than that of putrescine and spermidine; concentrations ranged from N.D. to 0.9 nM for cadaverine, and N.D. to 3.2 nM for norspermidine. Norspermine and spermine were detected in only a few samples; their concentrations varied from N.D. to 3.2 nM and N.D. to 0.5 nM, respectively. These concentrations were higher in the summer.     

胶州湾海水中溶解氨基酸的研究

于１９８６年１月－１１月用高效液相色谱法分析胶州湾１０个站位表层和底层海水中溶解游离氨基酸（ＤＦＡＡ）的组成、含量的分布及其季节变化。结果表明，７个站位的表层海水中月平均总溶解游离氨基酸（ＴＤＦＡＡ）含量范围为１．２４－２．２８ｕｍｏｌ／Ｌ。多数站位在２月份处于最低值（０．４ｕｍｏｌ／Ｌ），１１月份达最高值（５．０ｕｍｏｌ／Ｌ）。所测氨基酸中，Ｇｌｕ，Ｇｌｙ、Ａｒｇ、Ｌｅｕ，Ｏｒｎ，Ｓｅｒ等占优势     

Spatial variability of phytoplankton absorption coefficients and pigments off Baja California during November 2002

We have estimated the spatial variability of phytoplankton specific absorption coefficients (a* _ph ) in the water column of the California Current System during November 2002, taking into account the variability in pigment composition and phytoplankton community structure and size. Oligotrophic conditions (surface Chl < 0.2 mg m⁻³) dominated offshore, while mesotrophic conditions (surface Chl 0.2 to 2.0 mg m⁻³) where found inshore. The specific absorption coefficient at 440 [a* _ph (440)] ranged from 0.025–0.281 m²mg⁻¹ while at 675 nm [a* _ph (675)] it varied between 0.014 and 0.087 m²mg⁻¹. The implementation of a size index based on HPLC data showed the community structure was dominated by picoplankton. This would reduce the package effect in the variability of a* _ph (675). Normalized a _ph curves were classified in two groups according to their shape, separating all spectra with peaks between 440 and 550 nm as the second group. Most samples in the first group were from surface layers, while the second group were from the deep chlorophyll maximum or deeper. Accessory photoprotective pigments (APP) tended to decrease with depth and accessory photosynthetic pigments (APS) to increase, indicating the importance of photoprotective mechanisms in surface layers and adaptation to low light at depth. Samples with higher ratios of APP:APS (>0.4) were considered as phytoplankton adapted to high irradiances, and lower ratios (<0.26) as adapted to low irradiances. We found a good relationship between APP:APS and a* _ph (440) for the deeper layer (DCM and below), but no clear evidence of the factors causing the variability of a* _ph (440) in the upper layer.     

液相色谱法测定城市自来水中的苯并(a)芘

针对目前测定生活饮用水中的苯并(a)芘(简称Bap),采用的是国家标准《生活饮用水标准检验法》GB5750-85中的纸层析—荧光分光光度法,其准确度、精密度很难令人满意,提出了使用高效液相色谱法来定量检测城市自来水中的Bap。实验结果表明:该方法快速、准确,具有优异的重现性,线性范围为4.0～30.0 ng/L,线性系数为0.9999。日内(5 h)、日间(5 d)精密度均小于4.0%(n=5),Bap的回收率为89.0%～93.4%。由于Bap见光极容易分解,影响测定结果,因此采样后应尽快分析。     

Development of an online analyzer of atmospheric H2O2 and several organic hydroperoxides for field campaigns

An online automated instrument was developed for atmospheric measurements of hydroperoxides with separation and quantification of H₂O₂ and several organic hydroperoxides. Samples were trapped in aqueous solutions in a scrubbing glass coil. Analyses were performed on an HPLC column followed by para-hydroxyphenylacetic acid (POPHA) acetic acid and peroxidase derivatization and fluorescence detection. Analytical and sampling tests were performed on different parameters to obtain optimum signal-to-noise ratios, high resolution and collection efficiencies higher than 95% for H₂O₂ and organic hydroperoxides. The obtained performances show large improvements compared to previous studies. The sampling and analytical devices can be coupled providing an online analyzer. The device was used during two field campaigns in the Marseilles area in June 2001 (offline analyzer) and in July 2002 (online analyzer) at rural sites at low and high altitudes, respectively, during the ESCOMPTE and BOND campaigns. During the ESCOMPTE campaign, H₂O₂ was detected occasionally, and no organic hydroperoxides was observed. During the BOND campaign, substantial amounts of H₂O₂ and 1−HEHP+MHP were often detected, and two other organic hydroperoxides were occasionally detected. These observations are discussed.     

液相色谱法测定鱼肌肉中孔雀石绿、结晶紫及其代谢物

孔雀石绿(MG)和结晶紫(GV)曾作为渔药使用,在鱼体内可分别代谢为无色孔雀石绿(LMG)及无色结晶紫(LGV),具有潜在的致癌性,已被许多国家禁用。本文研究了同时检测孔雀石绿、结晶紫及其代谢物无色孔雀石绿和无色结晶紫的液相色谱方法,建立了检测前处理方法及色谱条件。经过液液萃取和丙基磺酸阳离子树脂纯化,采用C18分离柱后串联二氧化铅柱氧化衍生的方法,同时检测母体药物及其代谢物,回收率>70%,重复性的相对标准偏差<15%,定量限分别为2μg/kg及1μg/kg。经样品实测,在一份鲈鱼样品中检测到无色孔雀石绿残留97μg/kg。     

产河豚毒素菌株的筛选、鉴定及透析培养

河豚毒素(Tetrodotoxin, TTX)在镇静、镇痛、麻醉、戒毒等神经性疾病治疗方面效果显著且无致瘾性,因此具有极好的应用前景,但由于其从河豚体内提取的成本过高,所以难以大量推广应用。越来越多的证据表明TTX来源于河豚体内共生的微生物。我们从野生横纹东方鲀(Takifugu oblongus)肝脏中分离得到了一株产TTX较高的芽孢杆菌3G2(Bacillus sp. 3G2),通过ELISA和胶体金的方法检测到其发酵液TTX含量为35 ng/mL。将该菌株接种于专用透析培养器中,不断流加新鲜培养基实现连续培养,同时实现简化分离工艺,对发酵液进行小鼠生物活性检测、TTX试纸条检测,并通过河豚毒素抗体免疫共沉淀纯化得到TTX粗品后进行高效液相色谱鉴定均表明发酵液中含有TTX且含量较高。本研究通过筛选产TTX的优质菌株进一步了证实河豚毒素外源性假说,并初步验证了透析法生产河豚毒素的优越性,为后续商业应用提供实践性基础。     

基于反相C8色谱柱的海洋浮游藻色素高效液相色谱分析方法有效性验证

对一种海洋浮游藻色素高效液相色谱分析方法进行了有效性验证。该方法使用反相C8色谱柱,以甲醇、乙腈和丙酮为流动相,并在流动相中添加吡啶/醋酸溶液作为修饰剂改善色素峰的分离效果。结果表明,4种色素标准在一定的浓度范围内线性关系良好,叶绿素a的线性范围为189.6~18 960μg/L,叶绿素b为89.2~8 920μg/L,β,β-胡萝卜素为7.77~777.2μg/L,叶黄素为15.28~1 528μg/L。除β,β-胡萝卜素外各色素标准的回收率在不同浓度下均在90%以上,相对标准偏差也普遍低于5%。在4个参考藻种和123个胶州湾现场样品中共检测出37种色素,一些关键的特征色素均获得了良好的分离效果。该方法操作简便,具有分离度好、灵敏度高、重复性好、回收率高等优点,适用于培养的藻种和现场样品中的海洋浮游藻色素分析。