手性2—（2—吡啶基）—4—甲酯基—1,3—噻唑烷的合成及应用

不对称氢化硅烷化可实现由含碳碳或碳杂双键的化合物合成手性醇和手性腹，在石油化工、药物合成、生物碱等生物活性物质的合成等领域具有潜在的应用价值．90年代以来，不断有高活性、高选择性的手性催化剂的开发研究报道［‘－‘］，使不对称硅氢化研究成为催化科学的一个研究方向．我们开展了带有毗吹取代基的座隆烷类手性络合催化剂的研究工作D·‘’．a一毗院甲醛、L一半就氨酸甲酯盐酸盐、氯化环辛M烯合＃［Rh（COD）CI」。以及Ph2SIH。按文献［7j制备，苯乙酮为分析纯试剂．所用仪器有SP－－2305型气相色谱仪，170SX－FTIR型…     

(1R,2S)或(1S,2R)-1,2-二苯基-2-氨基乙醇衍生物手性配体的合成及其用于不对称催化反应

重点报道了以（１Ｒ，２Ｓ）或（１Ｓ，２Ｒ）－１，２－二苯基－２－氨基乙醇衍生物手性配体的合成及其用于不对称催化反应的研究，如去氢氨基酸的氢化、醛的乙基锌加成、酮的还原、活泼亚甲基化合物的烷基化、醛的硅腈化和瑞福马斯基反应等．研究了手性配体的结构、底物和反应条件等对上述反应的对映选择性和催化活性的影响．     

手性1—芳基—2,2—甲基—1,3—丙二醇

简要综述了手性１－芳基－２，２－二甲基－１，３－丙二醇及其衍生物在不对称合成中应用和反应，包括作为手性化学位移试剂、拆分试剂、辅助剂、配体和不对称合成中间体。     

（1R,2S）或（1S,2R）—1,2—二苯基—2—氨基乙醇衍生物手性配体的合成及其用于不

重点报道了以（１Ｒ，２Ｓ）或（１Ｓ，２Ｒ）－１，２－二苯基－２－氨基乙醇衍生物手笥配体的合成及其用于不对称催化反应的研究，如去氢氨基酸的氢化，醛的乙基锌加成，酮的还原，活泼亚甲基化合物的烷基化，醛的硅腈化和瑞福马斯基反应等。研究了手性配体的结构，底物和反件等对上述反应的对映造反性和催化活性的影响。     

用新的非水溶剂体系制备含磷纤维素衍生物

用新的非水溶剂体系制备含磷纤维素衍生物尤田耙，张兴元，沈晓煊，郭荷民，胡小铭（中国科学技术大学化学系合肥２３００２６）关键词非水溶剂，含磷纤维素衍生物，合成近年合成的一些纤维素衍生物被用作不对称合成的手性催化剂配体［１］、拆分光学异构体的色谱手性固定...     

5,6—二亚甲基双环[2.2.1]庚—2—醇及其衍生物的旋光与构型

从（－）－（１Ｓ，２Ｒ，４Ｓ）－５，６－二亚甲基双环［２．２．１］庚－２－醇（Ｉ）和（－）－（１Ｓ，２Ｓ，４Ｓ）－５，６－二亚甲基双环［２．２．１］庚－２－醇（Ⅱ）出发，合成了它们的醚类和取代苯甲酸酯类光学纯的衍生物。通过［α］Ｄ测定和构型分析，发现它们是含有３个手性碳（Ｃ１，Ｃ２和Ｃ４）的桥环化合物，其旋光性与构型的关系均符合可极化度多级圆球不对称性模型。     

（S）—α,α‘—二苯基—2—吡咯烷甲醇的简便合成

（S）－a，a’一二苯基一2一毗咯烷甲醇（1）是许多手性催化剂的合成前体’‘’，如手性呢隆硼试剂2，它能高度不对称地还原联基化合物［‘j．近年来有许多关于合成1的报道，但由于产率低，步骤多或者使用了高毒性光气［’j使大量制备方法受到限制．我们以L一脯氨酸为原料，采用不同的N一保护基因，高产率、简便地合成了化合物1．研究表明，不同N一保护基团对1的合成总产率有影响，其中PhCH。作保护基团时产率最低，但对光学纯度没有影响．陪叹烷酮是许多含毗咯环的天然产物的合成原料［‘j，在不对称合成中是一种功能较多的手性辅助基团…     

三[α—噻吩甲酰三氟丙酮]—9—[烷基亚胺基4,5—二氮杂芴[合铕（Ⅲ）…

报道了以α－噻吩三氟丙酮（ＨＴＴＡ）为第一配体，９－丁基亚胺基－４，５二氮杂芴［Ｌ１］和９－十八烷基亚胺基－４，５－二氮杂易［Ｌ２］为第二配体，与铕（Ⅲ）的两种新型二嗜性的强荧光配合物的合成，并用元素分析、紫外光谱、红外光谱、小角Ｘ射线衍射、荧光光谱和差热－热重谱对其进行了表征。得到了其组成和结构信息。     

μ—4,4‘—联吡啶桥联三核Cu（Ⅱ）配合物的合成和磁性

合成了３种以４，４’－联吡啶为配体的三核环状Ｃｕ（Ⅱ）配合物［Ｃｕ３（４，４＇－ｂｐｙ）３．（ｐｈｅｎ）３］（ＣｌＯ４）６．２Ｈ２Ｏ（１），［Ｃｕ３（４，４＇－ｂｐｙ），（ｂｐｙ）３］（ＣｌＯ４）６．Ｈ２Ｏ（２）和［Ｃｕ３９４，４＇－ｂｐｙ）３．（ＮＯ２－ｐｈｅｎ）３］（ＣｌＯ４）６．６Ｈ２Ｏ（３）。经元素分析，电导，ＩＲ，电子光谱，ＥＳＲ，磁化率等方法进行了表征，推定该配合物具有以４，４’－联吡     

羟丙基-β-环糊精的取代度和取代位置对毛细管电泳手性药物分离的影响

研究手性化合物的分离分析方法是当今国际分析化学领域研究的热点．毛细管电泳（CE）手性分离具有高效、快速、低耗等特点，近年来已取得很大进展［‘j．环糊精（CD）及其衍生物是CE手性分离使用最多的手性选择剂，其手性分离机理是基于手性化合物（客体）的2个对映体与环糊精分子（主体）形成的包合物的稳定常数不同，而这种差别主要取决于主客体分子之间的匹配性．因此，CD及其衍生物的分子结构，包括CD衍生物的取代度和取代位，置，对手性识别有很大影响．目前，有关CD及其衍生物作为手性选择剂的CE手性分离报道较多“‘，研究的主…     

Comparison of calculated and experimental flow velocities upstream from the sampling cone of an inductively coupled plasma mass spectrometer

Experimentally-determined flow velocities in the 6 mm upstream from the sampling cone of an inductively coupled plasma mass spectrometer were compared with velocities determined from a computer simulation of the flow and those calculated from a modified hemispherical sink model. The measured values and those from the simulation agreed within experimental error, but differed from the values calculated from the modified hemispherical sink model by as much as 30%. An empirical alternative to the modified hemispherical sink model is presented that allows for accurate calculation of flow properties upstream from the sampling cone under a range of plasma conditions.     

Cation-exchange separation of metals in dimethyl sulphoxide-aqueous hydrochloric acid media

The behaviour of bismuth, cadmium, copper, lead, silver, tin and zinc on a cation-exchange resin in a solvent system consisting of dimethyl sulphoxide, hydrochloric acid and water was studied. The distribution coefficients of these metal ions between liquid and resin were determined as functions of the concentration of dimethyl sulphoxide and of hydrochloric acid. On the basis of the distribution coefficients found, predictions were made as to the possibilities of separating these metals from mixtures. Such separations were confirmed experimentally for bismuth from lead, bismuth from copper, zinc from lead, lead from cadmium, silver from copper, silver from lead, lead from cadmium from zinc, bismuth from lead from zinc, and bismuth from zinc from copper.     

宁夏枸杞甜菜碱提取物高效液相色谱指纹图谱研究

建立宁夏枸杞甜菜碱提取物高效液相色谱指纹图谱,为鉴别不同来源的宁夏枸杞提供依据。以10批宁夏不同产地的宁夏枸杞主栽品种"宁杞Ⅰ号"样品建立枸杞甜菜碱提取物指纹图谱共有模式,采用"中药色谱指纹图谱相似度评价系统"软件进行数据处理,对15批不同来源的枸杞样品进行了分析。结果表明:8个特征峰构成了宁夏枸杞甜菜碱提取物的色谱指纹图谱,不同产地、不同品种的枸杞样品甜菜碱提取物指纹图谱存在差异;建立的枸杞甜菜碱提取物高效液相色谱(HPLC)指纹图谱对不同产地、不同品种枸杞的鉴别有参考价值。     

Effects of Variety and Growing Location on Physicochemical Properties of Starch from Sweet Potato Root Tuber

Three sweet potato varieties with purple-, yellow-, and white-fleshed root tubers were planted in four growing locations. Starches were isolated from their root tubers, their physicochemical properties (size, iodine absorption, amylose content, crystalline structure, ordered degree, lamellar thickness, swelling power, water solubility, and pasting, thermal and digestion properties) were determined to investigate the effects of variety and growing location on starch properties in sweet potato. The results showed that granule size (D[4,3]) ranged from 12.1 to 18.2 μm, the iodine absorption parameters varied from 0.260 to 0.361 for OD620, from 0.243 to 0.326 for OD680 and from 1.128 to 1.252 for OD620/550, and amylose content varied from 16.4% to 21.2% among starches from three varieties and four growing locations. Starches exhibited C-type X-ray diffraction patterns, and had ordered degrees from 0.634 to 0.726 and lamellar thicknesses from 9.72 to 10.21 nm. Starches had significantly different swelling powers, water solubilities, pasting viscosities, and thermal properties. Native starches had rapidly digestible starch (RDS) from 2.2% to 10.9% and resistant starch (RS) from 58.2% to 89.1%, and gelatinized starches had RDS from 70.5% to 81.4% and RS from 10.8% to 23.3%. Two-way ANOVA analysis showed that starch physicochemical properties were affected significantly by variety, growing location, and their interaction in sweet potato.     

关于空间判断失误的扎记Ⅳ.单斜晶系:从非心到有心空间群

报道了 12个从单斜无心修正为单斜有心的晶体结构。其中 1例从C2修正到C2 /m ,2例从P2 1 到P2 1 /c。 9例从Cc到C2 /c ,除Cc修正到C2 /c的 6例已见诸文献外 ,列出其余 6例在较高对称空间群下的原子坐标     

Capillary zone electrophoresis separation and collection of spermatozoa for the forensic analysis of sexual assault evidence

The processing of sexual assault kits (SAKs) relies on the genetic analysis of material extracted from swabs collected from the assault victim. A vital step in producing an identifiable DNA profile of the perpetrator is the effective separation of perpetrator (sperm) and victim (epithelial) DNA that have been isolated from the collected evidence. We report the use of capillary zone electrophoresis for the separation of intact sperm from whole and lysed epithelial cells in SAKs. The separated components are deposited into wells of a microtiter plate using a computer-controlled fraction collector, and quantitative PCR is used to verify the collection of sperm cells by targeted amplification of male DNA. We present results from simulated sexual assault samples that have been aged for up to 18 months, as well as vaginal swabs from authentic forensic kits. Components extracted from the vaginal swabs from the SAK comigrated with an aged semen sample at 6.25 ± 0.25 min. Epithelial cells migrated from 10-12 min, producing baseline resolution of the components. Sperm cells were collected in a microtiter plate for downstream analysis.     

一种天然纳米纤维捕鸟蛛丝的物理化学结构表征

蜘蛛丝作为功能性结构材料, 其独特的纤维成型方法与优良的结构和性能引起许多人的关注. 从20世纪80年代开始有关蜘蛛丝的研究报道日益增加[1]. 与高温高压下或由溶剂纺丝成型的合成纤维相比, 蜘蛛丝在空气中凝固成型, 丝纤维成型安全、无害, 从腹部若干不同吐丝器产生不同种类的丝具有不同的用途[2]. 蜘蛛拖曳丝(dragline silk)的比强度大于钢丝, 且具有较大的断裂伸长率(9%～30%)[3,4], 抗张强度1.1～1.4 GPa. 在相对湿度50%和应变速率100%/min的条件下, 模量值可达10～50 GPa. 在所有已知纤维品种中, 蜘蛛丝的断裂能是最高的. 此外, 蜘蛛丝在许多方面的综合性能优于最优良的人造纤维. 另外, 蜘蛛丝的细度为已知纤度最小的天然有机纤维, 这种高性能丝具有捕捉昆虫甚至鸟类的功能, 因此蜘蛛丝是具有特异功能的天然纤维材料. 目前, 蜘蛛丝结构和性能的研究主要包括其化学组成[5]、结晶结构[6,7]、结构模型[8,9]以及其NMR表征[10]等, 这些研究揭示了蜘蛛丝的氨基酸组成、分子量及其分布、结晶度、晶胞尺寸、链构象以及结构模型等. 这些研究主要集中在少数几种蜘蛛品种上, 如金色圆网织网蛛(Nephila clavipes)、十字圆蛛(A.diadematus)和大腹圆蛛(A.ventrocosus)等. 目前, 已知的蜘蛛种类大于30 000种[11], 以蜘蛛丝为例的生物大分子材料研究是一个挑战性的课题. 国内蜘蛛丝的研究仅有大腹圆蛛拖曳丝蛋白一级结构的研究报道[12,13]. 本文报道了广西捕鸟蛛丝的红外光谱、形貌结构和原子力显微镜的初步研究结果.     

Use of chemometric and geostatistical methods to evaluate pesticide pollution in the irrigation and drainage channels of the Ebro river delta during the rice-growing season

Data sets obtained from quantitative analysis of seventeen pesticides in water samples from a network of irrigation and drainage channels in the Ebro river delta (Catalonia, NE Spain) have been analysed by chemometric and geostatistical methods. Samples were taken at fourteen locations during the main rice-growing season, from May to August 2005. Principal-component analysis enabled investigation of the spatial and temporal distribution of the main pollution patterns caused by application of pesticides in the region under study. A first pesticide-contamination pattern from the Ebro river was differentiated from a second more specific pattern from the water-drainage channels of the delta, collected from the rice fields. The seasonal peak in this more specific rice pesticide source was observed in July. Coupling the results from chemometric data analysis with use of geostatistical methods was shown to be a useful procedure for discovery of the most significant spatial and monthly variations of the main pesticide-contamination patterns, taking into account the particular geographical structure of the area under study.     

人尿中氟含量的测定及其意义

采用氟离子选择电子法对右江民族医学院28名≥19岁的成年健康学生(其中男生18名,女生10名)早上和晚上尿样分别进行了氟含量测定。结果表明,早上和晚上尿样尿氟含量有一定差异,而早上尿样中的氟含量小于晚上尿样。可认为从早到晚的时段内,人体从食物、水源或其它途径摄入了氟,从而出现了差异;样品氟含量的最大值0.959 mg/L在百色地区正常人尿氟百分位数法(P25～P97.5)正常值范围0.589～2.268 mg/L内,可认为右江民族医学院的人员未出现氟中毒,处于一个氟安全的地区。     

The Influence of Bacteria Causing Subclinical Mastitis on the Structure of the Cow’s Milk Microbiome

Mastitis is the most expensive disease of dairy cattle across the world and is the main reason for the use of antibiotics in animal husbandry. The aim of this study was to analyze the microbiome of raw milk obtained from a semi-subsistence farm located in the Kuyavian–Pomeranian Voivodeship in Poland. Milk from healthy cows and from cows with subclinical mastitis was analyzed. The following pathogenic bacteria were found in milk from individuals with subclinical mastitis: Escherichia coli or Streptococcus agalactiae. The composition of drinking milk was assessed on the basis of 16S rRNA gene sequencing using the Ion Torrent platform. Based on the conducted research, significant changes in the composition of the milk microbiome were found depending on the physiological state of the cows. The microbiome of milk from healthy cows differed significantly from the milk from cows with subclinical mastitis. Two phyla dominated in the milk from healthy cows: Firmicutes and Proteobacteria, in equal amounts. On the contrary, in the milk from cows with diagnosed subclinical mastitis, one of the types dominated: either Firmicutes or Proteobacteria, and was largely predominant. Moreover, the milk microflora from the ill animals were characterized by lower values of the determined biodiversity indicators than the milk from healthy cows. The presence of pathogenic bacteria in the milk resulted in a significant reduction in the share of lactic acid bacteria in the structure of the population of microorganisms, which are of great importance in the production technology of regional products.