Na－Ca－Ba－RE氟碳酸盐系列矿物的两个新变种

Ｃａ氟碳钡铱矿富Ｓｒ变种和白云鄂博矿富Ｃａ变种分别产于俄罗斯科拉半岛希宾碱性岩体的碳酸盐和内蒙古白云鄂博钥铁稀土矿床碳酸盐脉石中。据电子探针分析得到的晶体化学式分别为：（Ｃ３＿（０．４６），Ｎａ＿（０．２８），□＿（０．１６））＿（０．９０）Ｂａ＿（１．０３）（Ｃｅ＿（０．８２），Ｓｒ＿（０．３８），Ｌａ＿（０．３５），Ｎｄ＿（０．３２），Ｐｒ＿（０．０９），Ｓｍ＿（０．０１））＿（１．９７）（ＣＯ＿３）＿４Ｆ和（Ｎａ＿（０．４４），Ｃａ＿（０．３２），□＿（０．２４））＿（１．００）Ｂａ＿（１．０７）（Ｃｅ＿（１．０３），Ｌａ＿（０．４６），Ｎｄ＿（０．２６），Ｐｒ＿（０．０８），Ｓｒ＿（０．０８），Ｓｍ＿（０．０２））＿（１．９３）（ＣＯ＿３）＿４Ｆ。由Ｘ射线方法测定的晶胞参数分别是：ａ＝０．５０９１，ｃ＝２．３０２ｎｍ和ａ＝０．５１１０，ｃ＝０．３３３ｎｍ。二者是Ｃａ氟碳钡铈矿（Ｃａ＿（０．５），□＿（０．５））ＢａＣｅ＿２（ＣＯ＿３）＿４Ｆ和白云鄂博矿ＮａＢａＣｅ＿２（ＣＯ＿３）＿４Ｆ类质同象系列的中间成员。基于白云鄂博矿晶体结构中离子半径的分析和键价的计算，表明Ｃａ＿￣（２＋）优先占据Ｎａ位，而Ｓ     

气相色谱法测定恶性血液病患者血浆中游离脂肪酸的含量

应用气相色谱法测定了恶性血液病患者（急性淋巴细胞性白血病、急性粒细胞性白血病、淋巴瘤）血浆中主要游离脂肪酸（Ｃ＿（１６：０）,Ｃ＿（ｌ８：０）,Ｃ＿（１８：１）,Ｃ＿（ｌ８：２））的浓度。所有恶性血液病患者血浆中几个主要的游离脂肪酸浓度,大多数比正常值显著降低（Ｐ＜０．０５或Ｐ＜０．０１）。     

Gd_xY_（1－x）P_5O_（14）：Ce，Tb的发光和能量传递Ⅱ．Ce→

研究了Ｇｄ＿ｘＹ＿（１－ｘ）Ｐ＿５Ｏ＿（１４）：Ｃｅ＿（０．０１），Ｔｂ＿（０．０２）体系中Ｇｄ的子晶格在Ｃｅ→Ｇｄ→Ｔｂ能量传递中的中介作用规律及ＧｄＰ＿５Ｏ＿（１４），ＧｄＰ＿５Ｏ＿（１４）：Ｃｅ，ＧｄＰ＿５Ｏ＿（１４）：Ｔｂ和Ｇｄ＿ｘＹ＿（１－ｘ）Ｐ＿５Ｏ＿（１４）：Ｃｅ，Ｔｂ的荧光光谱、激发光谱。结果表明，当ｘ＞０．７时，结构从单斜Ⅱ（Ｃ２／ｃ）的层状结构变为单斜Ｉ（Ｐ２＿１／ｃ）的带状结构，Ｃｅ￣（３＋）的发射光谱和Ｇｄ￣（３＋）的吸收光谱交迭增加等是Ｃｅ￣（３＋）→Ｇｄ￣（３＋）→Ｔｂ￣（３＋）能量传递几率增加的主要原因。     

关于液相色谱保留值公式的补充

本文介绍了液相色谱保留值公式研究的历史,根据色谱保留值公式的统一形式运用液相吸附公式得到ｌｎｋ＇＝Ａ＋Ｂｌｎ（Ｃ＿（Ｂ＿１）／θ＿（Ｂ＿１））＋ＣＣ＿（Ｂ＿１）。当强溶剂浓度Ｃ＿（Ｂ＿１）不至太低时有ｌｎｋ＇≈Ａ＋ＢｌｎＣ＿（Ｂ＿１）＋ＣＣ＿（Ｂ＿１）：作者证明了当强溶剂浓度Ｃ＿（Ｂ＿１）→０时,ｋ＇→常数,从而纠正了长期存在于色谱热力学理论中Ｃ＿（Ｂ＿１）→０,ｋ＇→∞的谬误。     

NdSr_（1－x）M_xNiO_4（M＝Ca，Ba）的合成，结构和电学磁学性

用固相法首次合成了ＮｄＳｒ＿（１－ｘ）Ｍ＿ｘＮｉＯ＿４（Ｍ＝Ｃａ：０．０≤１．０；Ｍ＝Ｂａ：０．０≤ｘ≤０．６）系列复合氧化物，并研究了其结构，红外光谱，电学性质和磁学性质。除ＮｄＣａＮｉＯ以正交晶系结晶外，其它试样的结构均属于四方晶系。ＩＲ谱显示随Ｃａ￣（２＋）离子含量的增加，ＮｄＳｒ＿（１－ｘ）Ｍ＿ｘＮｉＯ＿４的Ｎｉ－Ｏ键缩短，Ｃａ￣（２＋）和Ｂａ￣（２＋）引入ＮｄＳｒＮｉＯ＿４以取代Ｓｒ￣（２＋），使试样由金属性导电转变为半导体性导电；随Ｃａ￣（２＋）含量增加，试样的室温电阻率增大。７７～３００Ｋ磁化率与温度关系曲线显示，所有试样的Ｎｉ￣（３＋）都以低自旋状态存在。     

（CeO_2）_（0．7－x）（MO）_x（La_2O_3）_（0．3）（M＝

合成了（ＣｅＯ＿２）＿（０．７－ｘ）（ＭＯ）＿ｘ（Ｌａ＿２Ｏ＿３）＿（０．３）（Ｍ＝Ｍｇ、Ｃａ、Ｓｒ）固体电解质。对其晶体结构、电导率、ＸＰＳ谱、离子迁移数及制成的燃料电池的Ｖ－Ｉ曲线进行了测定。（ＣｅＯ＿２）＿（０．７）（Ｌａ＿２Ｏ＿３）＿（０．３）中掺入Ｃａ￣（２＋）、Ｍｇ￣（２＋）或Ｓｒ￣（２＋），可使电解质的氧离子导电性能改善，从而使制成的燃料电他的开路电压输出功率也得到提高。     

低碳醇合成Raney Cu－Co催化剂的研究Ⅰ．反应性能考察

本文在５６３Ｋ、６ＭＰａ及Ｈ＿２／ＣＯ＝２的条件下，考察了Ｃｕ／Ｃｏ比不同的几个ＲａｎｅｙＣｕ－Ｃｏ催化剂的反应性能。结果表明：ＲａｎｅｙＣｕ－Ｃｏ催化剂上ＣＯ加氢产物主要为Ｃ＿１－Ｃ＿６正构醇及Ｃ＿１－Ｃ＿８正构烃。烃和醇产品的分布均符合Ｓｃｈｕｌｚ－Ｆｌｏｒｙ方程。但醇产品的链增长几率（０．３－０．５５）均小于烃产品的值（０．６－０．７５）。Ｃｕ／Ｃｏ比不同的催化剂在进入活性稳定区之前，均经过了一个不尽相同的活性波动区，活性趋于稳定所需时间随Ｃｕ／Ｃｏ比增大而缩短。Ｃｕ／Ｃｏ＝０．３－１．５（原子比）时，就醇收率而言，ＲａｎｅｙＣｕ－Ｃｏ催化剂明显高于共沉淀Ｃｕ－Ｃｏ催化剂，Ｃｕ／Ｃｏ＝０．８（原子比）时，稳定醇收率达０．５７ｇ·ｇ￣（－１）·ｈ￣（－１）。     

非离子表面活性剂层状液晶的结构与增溶作用

相行为研究表明，与ＴｒｉｔｏｎＸ－１００／Ｃ＿６Ｈ＿６／Ｈ＿２Ｏ体系相比，ＴｒｉｔｏｎＸ－１００／Ｃ＿（１０）Ｈ＿（２１）ＯＨ／Ｈ＿２Ｏ体系更易于生成层状液晶，并更为稳定，小角Ｘ－射线衍射表明；ＴｒｉｔｏｎＸ－１００／Ｃ＿（１０）Ｈ＿（２１）ＯＨ／Ｈ＿２Ｏ体系层状液晶中，Ｃ＿（１０）Ｈ＿（２１）ＯＨ与ＴｒｉｔｏｎＸ－１００交替排列于两亲双层中，Ｃ＿（１０）Ｈ＿（２１）ＯＨ／ＴｒｉｔｏｎＸ－１００重量比增加，两亲双层厚度ｄ＿０值不变。以Ｃ＿６Ｈ＿６代替Ｃ＿（１０）Ｈ＿（２１）ＯＨ后，Ｃ＿６Ｈ＿６存在于两亲双层的油层和渗入ＴｒｉｔｏｎＸ－１００分子链尾周围，使得溶剂渗透率减少，并且Ｃ＿６Ｈ＿６／ＴｒｉｔｏｎＸ－１００增加，ｄ＿０值增加。     

微分电位溶出法测定人发中铜铅镉锌的研究

本文报道了０．００２５ｍｏｌ·Ｌ￣（－１）ＨＣｌ－０．２ｍｏｌ·Ｌ￣（－１）ＮＨ＿（４）Ｃｌ底液中连续测定人发中铜、铅、镉、锌的微分电位溶出法。四元素峰电位分别为－０．２０Ｖ，－０．４６Ｖ，－０．６７Ｖ，一１．０２Ｖ（ＳＣＥ），峰形好，灵敏度高，干扰少，测定发样相对标准偏差≤４．３％，回收率为９７．６％～１０４．６％。并对ＨＮＯ＿３－ＨＣｌＯ＿４和ＨＮＯ＿（３）Ｈ＿（２）Ｏ＿２消化发样进行了比较。     

铜（Ⅱ）锌（Ⅱ）－氟哌酸体系电化学行为及示波极谱法研究

铜（Ⅱ）和锌（Ⅱ）分别在０．１ｍｏｌ／ＬＫＨ＿２ＰＯ＿４－Ｎａ＿２ＨＰＯ＿４缓冲溶液（ｐＨ６．５）和０．２５ｍｏｌ／ＬＮＨ＿４Ｃｌ溶液中，与氟哌酸形成良好的络合吸附波，峰电位分别为－０．２６Ｖ和－１．２８Ｖ（ｖｓ；ＳＣＥ）；络合比分别为１：３和１：２；峰电流与铜（Ⅱ）和锌（Ⅱ）的浓度均在４．０×１０￣（－７）～５．０×１０￣（－６）ｍｏｌ／Ｌ范围内呈线性关系，检测限分别为７．０×１０￣（－８）和５．０×１０￣（－８）ｍｏｌ／Ｌ。用线性扫描和循环伏安法等手段研究体系的行为，表明均具吸附性，而铜（Ⅱ）－氟哌酸体系属络合物中铜（Ⅱ）的两电子还原的可逆过程。     

毛细管气相色谱法鉴定分析杆菌

本文利用ＯＶ－１０１熔融石英毛细管柱，对１５种标准分枝杆菌的色谱特征进行了研究，得到了特异性指纹图。并对４２株临床菌株进行了鉴别。     

气相色谱法鉴别缓慢生长分枝杆菌

采用毛细管气相色谱法对９种缓慢生长分枝杆菌的化学成分进行了分析。结果表明,不同菌种的色谱图存在明显的差异。对７５株临床菌株进行色谱法鉴别,并与传统生物学鉴定法作了对比。     

Fast identification of mycobacterium species by GC analysis with trimethylsulfonium hydroxide (TMSH) for transesterification

Trimethylsulfonium hydroxide (TMSH) reproducibly converts fatty acids bound in, e.g., biomolecules such as phospholipids and/or glycerides, into the corresponding fatty acid methyl esters (FAMEs). The transesterification can be performed at room temperature in a fast single step reaction. Surprisingly, secondary alcohols and mycolic acid cleavage products (MACPs) are also released from mycobacteria under these conditions. The complex reaction mixtures containing FAMEs, MACPs, and secondary alcohols can easily be separated by high resolution temperature-programmed capillary GC. Different species of mycobacteria give rise to characteristic chromatographic patterns and the amount of lipids from a single colony of mycobacteria is sufficient for reliable identification of the bacteria. The profiles of the chromatograms match well those obtained from other sample preparation techniques. The TMSH method of identification of mycobacteria from the patterns of the gas chromatograms is faster and more sensitive than conventional methods, which also involve transesterification. The identification of mycobacterial species by microbiological culture techniques is difficult to perform and requires several weeks.     

Stereoselectivity in the synthesis of polyprenylphosphoryl β-d-ribofuranoses

Decaprenylphosphoryl β-d-arabinofuranose (DPA) is a key arabinose donor in mycobacteria. The ribo analog of DPA (DPR) has also been found in mycobacteria. It has recently been confirmed that DPA is formed via a two-step epimerization of DPR. The stereoselective synthesis of DPR as well as two shorter analogs of DPR is described.     

A Metabolic-Tag-Based Method for Assessing the Permeation of Small Molecules Across the Mycomembrane in Live Mycobacteria**

The general lack of permeability of small molecules observed for Mycobacterium tuberculosis (Mtb) is most ascribed to its unique cell envelope. More specifically, the outer mycomembrane is hypothesized to be the principal determinant for access of antibiotics to their molecular targets. We describe a novel assay that combines metabolic tagging of the peptidoglycan, which sits directly beneath the mycomembrane, click chemistry of test molecules, and a fluorescent labeling chase step, to measure the permeation of small molecules. We showed that the assay workflow was robust and compatible with high-throughput analysis in mycobacteria by testing a small panel of azide-tagged molecules. The general trend is similar across the two types of mycobacteria with some notable exceptions. We anticipate that this assay platform will lay the foundation for medicinal chemistry efforts to understand and improve uptake of both existing drugs and newly-discovered compounds into mycobacteria.     

Developing rapid detection of mycobacteria using microwaves

In this paper, we describe the development of a culture-based biochip device for rapid detection of mycobacteria in environmental samples. Individual biochips rely upon the unique paraffinophilic nature of mycobacteria to rapidly and selectively adhere to the surface of the device. We used prototype biochips to experimentally demonstrate the concept of rapid and selective detection of mycobacteria by testing pure cultures and using epifluorescence microscopy to visualize microorganisms on the surface. As an alternative, rapid approach for identifying the biomass on the biochip surface, we used microwaves in the 10 to 26 GHz frequency range. The results of this study indicate that different microorganisms are responsible for specific shifts in resonance frequencies of a microwave cavity. By combing the semi-selective paraffin surface of the biochip with the microorganism-specific response to the microwaves, we have developed an improved analytical system with the potential to rapidly identify and enumerate mycobacteria in environmental samples in as little as 2 h.     

MmpL genes are associated with mycolic acid metabolism in mycobacteria and corynebacteria

Mycolic acids are vital components of the cell wall of the tubercle bacillus Mycobacterium tuberculosis and are required for viability and virulence. While mycolic acid biosynthesis is studied extensively, components involved in mycolate transport remain unidentified. We investigated the role of large membrane proteins encoded by mmpL genes in mycolic acid transport in mycobacteria and the related corynebacteria. MmpL3 was found to be essential in mycobacteria and conditional depletion of MmpL3 in Mycobacterium smegmatis resulted in loss of cell wall mycolylation, and of the cell wall-associated glycolipid, trehalose dimycolate. In parallel, an accumulation of trehalose monomycolate (TMM) was observed, suggesting that mycolic acids were transported as TMM. In contrast to mycobacteria, we found redundancy in the role of two mmpL genes, in Corynebacterium glutamicum; a complete loss of trehalose-associated and cell wall bound corynomycolates was observed in an NCgl0228-NCgl2769 double mutant, but not in individual single mutants. Our studies highlight the role of mmpL genes in mycolic acid metabolism and identify potential new targets for anti-TB drug development.     

Detection of Mycobacterium leprae in Formalin-Fixed Paraffin-Embedded Sample by Fite-Faraco Staining and Polymerase Chain Reaction

Leprosy is a chronic infectious disease caused by Mycobacterium leprae. The identification of mycobacteria in tissue sections can be made through a microscopic examination with fite-faraco staining or PCR method. Paraffin blocks from four patients with leprosy were retrieved from The Pathologic Department of Dr.Soetomo Hospital, Surabaya. Two cases were from paucibacillary leprosy patients with no mycobacteria stained by fite-faraco. PCR assay showed a negative result. The other two cases were multibacillary leprosy with many bacteria stained by fite-faraco. PCR assay showed a positive result.     

Impact of updating the MALDI‐TOF MS database on the identification of nontuberculous mycobacteria

Conventional identification of mycobacteria species is slow, laborious and has low discriminatory power. Matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOF MS) has proved highly effective for identifying conventional bacteria, and it may also be useful for identifying mycobacteria. The aim of this study was to evaluate and compare MALDI‐TOF MS with currently recommended molecular methods for the identification of nontuberculous mycobacteria (NTM), applying Mycobacteria Libraries v3.0 (ML3.0) and v2.0 (ML2.0). A total of 240 clinical isolates of 41 NTM species grown on solid media were analysed: 132 isolates of slow‐growing mycobacteria and 108 of rapid‐growing mycobacteria. MALDI‐TOF MS, using ML3.0, identified 192 (80%) NTM isolates with a score ≥1.7, encompassing 35 (85.4%) different species, that is, 17 (7.1%; p  = 0.0863) isolates and 15 (36.6%; p  = 0.0339) species more than currently recommended molecular techniques (polymerase chain reaction reverse hybridization). All these isolates were correctly identified according to molecular identification methods. The application of ML3.0 also identified 15 (6.2%) NTM isolates more than ML2.0 (p  < 0.01). The scores obtained with MALDI‐TOF MS using ML3.0 (mean score: 1.960) were higher in 147 (61.2%) isolates than when using ML2.0 (mean score: 1.797; p  < 0.01). Three of the species analysed were not included in either database, so they were not recognized by this system. In conclusion, MALDI‐TOF MS identified more isolates and species than the recommended polymerase chain reaction reverse hybridization assays. Although the new ML3.0 is not the definitive database, it yielded better results than ML2.0. This shows that the updating of the MALDI‐TOF MS database plays an essential role in mycobacterial identification. Copyright © 2017 John Wiley & Sons, Ltd.     

Characterization of mycobacterial triacylglycerols and monomeromycolyl diacylglycerols from Mycobacterium smegmatis biofilm by electrospray ionization multiple-stage and high-resolution mass spectrometry

The storage of triacylglycerols (TAGs) is essential for non-replicating persistence relevant to survival and the re-growth of mycobacteria during their exit from non-replicating state stress conditions. However, the detailed structures of this lipid family in mycobacteria largely remain unexplored. In this contribution, we describe a multiple-stage linear ion-trap mass spectrometric approach with high resolution mass spectrometry toward direct structural analysis of the TAGs, including a novel lipid subclass previously defined as monomeromycolyl diacylglycerol (MMDAG) isolated from biofilm of Mycobacterium smegmatis, a rapidly growing, non-pathogenic mycobacterium that has been used as a tool for molecular analysis of mycobacteria. Our results demonstrate that the major isomer in each of the molecular species of TAGs and MMDAGs consists of the common structure in which Δ⁹18:1- and 16:0-fatty acyl substituents are exclusively located at sn-1 and sn-2, respectively. Several isomers were found for most of the molecular species, and thus hundreds of structures are present in this lipid family. More importantly, this study revealed the structures of MMDAG, a novel subclass of TAG that has not been previously reported by direct mass spectrometric approaches.