二十碳五烯酸甲酯标准样品的研制

以深海鱼油为基础原料,将其皂化水解为游离脂肪酸,经尿素—甲醇包合粗分离后,以硫酸—甲醇甲酯化,再经硝酸银—硅胶柱层析精分离,得到高纯度的二十碳五烯酸甲酯标准物质。经定值检测,确定其化合物纯度≥98%。     

顶空固相微萃取气相色谱质谱嗅觉测量联用初探鲢肉的挥发性风味物质

为探明鲢肉挥发性气味特征物质,通过顶空固相微萃取法提取和浓缩了鲢肉中的挥发性物质,并利用气相色谱质谱联用以及气相色谱〖CD*7/9〗嗅觉测量法对气味物质进行了定性分析及气味特征的评价。由8人组成的评价小组通过检测频率法进行嗅觉测量。结果表明,经GCMS分析鉴定得到了29种挥发性气味物质,主要是一些羰基类和醇类化合物,占了总挥发性物质的88%。通过检测频率分析法鉴定出12种化合物具有气味特征,表现为鱼腥、金属、青草、油脂氧化、蘑菇等特征。另外有4种未知物也显示了较强的风味特性,它们协同作用构成了鲢的特殊气味。     

气相色谱法测定水产品中氯霉素残留

介绍了水产品中氯霉素残留量测定的气相色谱法。样品中的氯霉素用乙酸乙酯提取,正己烷去脂肪,过Sep-C18柱进行净化,用BSTFA-TMCS衍生后进带有微电子俘获器的气相色谱仪检测。该方法的线性范围为0.5～500μg·L-1,相关系数r=0.999,最低检测限为0.1μg·kg-1,相对标准偏差为4.3%～11.0%,向样品中分别添加1μg·kg-1、10μg·kg-1和20μg·kg-13个浓度水平的氯霉素,回收率分别为62.0%、88.2%和96.4%。方法灵敏度高,准确可靠,适合水产品中氯霉素残留量的检测。     

美洲鲥仔稚鱼脊柱及附肢骨骼系统的早期发育

使用软骨-硬骨双染色技术,描述了美洲鲥(Alosa sapidissima)仔稚鱼(1~51日龄)脊柱、胸鳍、尾鳍、背鳍等附肢骨骼的形态发育特征。结果显示,脊柱的发育开始于10日龄仔鱼尾部的髓弓、脉弓和尾下骨的出现,16日龄髓弓和脉弓延伸形成髓棘和脉棘,19日龄脊柱出现分节的硬骨环,23日龄所有椎体形成。各附鳍支鳍骨发育顺序先后依次为胸鳍、尾鳍、背鳍、臀鳍和腹鳍。胸鳍在2日龄时出现乌喙骨,13日龄形成软骨质的胸鳍支鳍骨,19日龄仔鱼肩带和上匙骨开始骨化;尾鳍的尾下骨最早出现在5日龄,12日龄尾鳍形成2枚尾上骨、1枚尾杆骨和6枚尾下骨,19日龄仔鱼尾椎和尾鳍率先开始骨化,直至23日龄尾鳍骨骼系统钙化完全。最终背鳍和臀鳍分别形成18和22根鳍条。美洲鲥骨骼发育研究对其早期发育功能趋向、环境优化及分类鉴定有重要作用。     

芦笋中毒死蜱和氯氰菊酯残留的同时测定

采用乙腈提取,Florisil固相萃取,正己烷-丙酮洗脱,HP-5石英柱程序升温技术分离,电子捕获检测器检测,建立了同时测定芦笋中毒死蜱和氯氰菊酯残留量的固相萃取-毛细管气相色谱法。结果表明,该方法对2种农药残留量的线性范围分别为0.002 5-0.500 0 mg/L和0.005-0.250 mg/L,相关系数为0.999 8-0.999 9,检出限分别为0.002 5 mg/kg和0.005 mg/kg,加标平均回收率为74.0%-98.3%,相对标准偏差为0.6%-10.8%。     

半解析法求解水柱分离与断流弥合水锤问题及机理分析

为了应对长距离输水工程的水锤防护问题,分析了空气阀作用于波状管线有压输水系统发生水力过渡时的瞬态响应过程,提出了空穴增长和溃灭时间、管线最大含气率、最大压力峰值等参数的半解析公式,并由此探讨和研究影响空气阀水锤防护效果的关键因素。半解析解表明,位于空气阀下游的管段相对长度和管线高点的相对高程对系统的断流弥合水锤起了主导作用。将半解析解与特征线法数值解进行了对比,发现两者随主变量的变化趋势一致;分析了半解析解与数值解产生偏差的原因与半解析公式推导过程中几个假设的关系。结果证明,该文提出的半解析公式能够反映空气阀作为水锤防护装置时,主导断流弥合水锤压力峰值的关键因素。该研究可为水锤防护的相关研究提供参考。     

再生水灌溉对土壤理化性质影响的试验研究

通过室内土柱模拟试验的方法，研究了再生水灌溉对土壤理化性质的影响。结果表明：再生水灌溉对土壤扩散率和饱和导水率的影响与连续灌溉再生水的次数有关，短时间灌溉有降低的作用，但随着灌溉次数的增加，土壤扩散率和饱和导水率有增加的趋势；同时，随着灌溉次数的增加，土壤pH值降低，土壤有机质和全盐量增加；土壤溶液中各离子浓度有显著变化。灌溉5次之后，除0～10cm土层全盐量为0．107％外，其他各层均低于0．1％的限度；0～10，10～20，30～40cm土层的ESP均在5％～10％范围之内，20～30cm土层的ESP基本保持在原始的水平。再生水灌溉对土壤次生盐渍化的影响不显著。     

干柱层析法制备油茶总皂苷对照品初探

目的 研究干柱层析法制备油茶皂苷对照品的方法。方法 原料用60 %乙醇超声提取,浓缩至无醇味,石油醚脱酯后用正丁醇按3:1体积比加入萃取。取正丁醇层并真空浓缩至干,干法上样于100目~200目硅胶柱色谱分离,用乙酸乙酯-甲醇-正丁醇-水(2:1:4:7)的上相展层;根据Rf值取出相应的条带并用甲醇淋洗收集蒸干,薄层及理化性质检测。结果 该方法所制样品由薄层色谱为一点,纯度较高。结论 该方法简便、实用且制备量大,可作为油茶总皂苷对照品。     

酿酒酵母菌胞内海藻糖提取工艺参数的优化

建立了超声破碎酿酒酵母细胞和冷三氯乙酸化学浸提海藻糖的工艺，探索了离子色谱分析技术条件，采用响应曲面法（RSM），研究了液料比R、超声功率W、工作时间T1、超声总时间T2和浸提时间T3等5个试验关键因子对海藻糖提取的影响规律，并构建了动态控制的数学模型，得到了海藻糖提取最优工艺参数依次为：尺为7、W为698W、T1为4．9s、T2为7．3min、T3为9min。结果表明：模型极显著，具有可行性和有效性，超声功率、工作时间和超声总时间对海藻糖提取量的影响最大，为生产中的应用提供了科学依据。     

Characterization of humus-protease complexes extracted from soil

Pyrophosphate (140 mM, pH 7.1) extracts of two arable soils and one pasture soil were ultrafiltrated separating the extracted material into three fractions: A_I with nominal molecular weight (nmw) > 100 kD, A_II with nmw between 10 kD and 100 kD and R with nmw < 10 kD. Protease activity was determined in the fractions by using three different substrates: N-benzoyl-l-argininamide (BAA), specific for trypsin; N-benzyloxy-carbonyl-l-phenylalanyl l-leucine (ZPL), specific for carboxypeptidases; and casein, essentially a non-specific substrate. The derivative fractions were also analysed for their amino acid N and humic (HA) and fulvic (FA) acid contents. The organic matter of extracts and derivative fractions obtained from the pasture soil was analysed by isoelectric focusing (IEF) and that of fractions analysed by pyrolysis gas chromatography (Py-GC). Activities of the extract were monitored for their thermal stability and those of the extract and derivative fractions for their optimal pH.Due to the mechanical disintegrating action of sodium pyrophosphate over the humic substances during the fractionation process the amount of total organic C and FA in the fractions was ranked as R > A_II > A_I. The lowest amino acid N/organic C was found in the R fraction, whereas A_II fraction was rich in humic acids, carbohydrates and amino acid N and A_I fraction showed the lowest carbohydrate content. At least 70% of the total BAA- and ZPL-hydrolysing activity was associated to particles with nmw higher than 10 kD and at least 30% of these activities were present in particles with nmw higher 100 kD. Casein-hydrolysing activity was quite evenly distributed among the three fractions (A_I, A_II and R). The extracted protease-organic complexes were resistant to thermal denaturation and some of them showed optimal activity at pH values higher than 10 as a result of the polyanionic characteristics of the humic material surrounding enzyme molecules and of the presence of alkaline protease. Comparison of data obtained in Py-GC analyses and in protease activity suggests that BAA-hydrolysing activity was associated to a highly condensed humic matter and ZPL-hydrolysing activity to less resistant humic substances, while at least some of the extracted casein-hydrolysing activity was present as glyco-proteins not associated to humus. BAA-hydrolysing activity was probably inhibited by fresh organic matter of carbohydrate origin whereas lignin derived organic matter probably inhibited ZPL- and casein-hydrolysing activity.