腹腔注射稀土化合物对小鼠肝脏抗氧化酶活性和脂质过氧化水平的影响

成年小鼠每天腹腔注射０．２８ｍｍｏｌ／ｋｇ剂量的ｔｏＣｌ３、Ｌａ－ＤＴＰＡ、ＴｂＣｌ３和Ｔｂ－ＤＴＰＡ生理盐水溶液，连续三天后与生理盐水对照组比较，ＬａＣｌ３使小鼠肝脏脂质过氧化（ＬＰＯ）水平升高，超氧歧化酶（ＳＯＤ）活性降低，而ＴｂＣｌ３的影响不明显；ＬａＣｌ３和ＴｂＣｌ３均显著降低谷恍甘肽过氧化酶（ＧＳＨ－Ｐｘ）活性。同样剂量Ｌａ－ＤＴＰＡ和Ｔｂ－ＤＴＰＡ对上述三项指标基本无影响。     

邻苯二胺—过氧化氢—辣根过氧化物酶酶联免疫示差脉冲伏安法测定人血清…

建立了邻苯二胺（ＯＰＤ）－Ｈ２Ｏ２－辣根过氧化物酶（ＨＲＰ）酶联示差脉冲伏安分析体系并用于测定人血清中类风湿因子（ＲＦ），ＨＲＰ催化Ｈ２Ｏ２氧化ＯＰＤ所形成麦催化产物在ＰＨ２．０磷酸盐－枸椽酸缓冲溶液中于－０．１８Ｖ左右产生－灵敏示差脉冲伏安峰，在ＲＦ浓度在１．２５－２０．０Ｕ／ｍＬ之间与峰电流呈线性关系，应用此峰检测人血清ＲＦ的检测限低至０．２８Ｕ／ｍＬ。该法较相同条件下ＥＬＩＳＡ以光度测定法的     

二溴羟基苯基荧光酮荧光猝灭法测定Br^—

本文报道了以二溴羟基苯基荧光酮（ＤＢＨ－ＰＦ）为指示剂，在阳离子表活性剂ＣＰＣ存在下荧光猝灭间接测定Ｂｒ＾－的新方法。在０．６ｍｏｌ／ＬＨ２ＳＯ４介质中，Ｂｒ＾－和ＢｒＯ３＾－反应生成Ｂｒ２，Ｂｒ２与ＤＢＨ－ＰＦ（λｅｍ＝５２０ｎｍ）生成红色化合物，使体荧光猝灭。Ｂｒ＾－含量在０．２５－６．２５μｇ／２５ｍＬ范围内有良好的线性关系，检测限为０．２５μｇ／２５ｍＬ。该法灵敏度高，选择性好，用于合成海     

高效液相色谱法测定羊体内的丙硫咪唑缓释弹代谢产物的血药浓度

用反相高效液相色谱法追踪分析不同时间内羊血清中药物浓度的变化，以供药物代谢动力学研究。药物为丙硫咪唑砜和丙硫咪唑亚砜（简称砜和亚砜），实验条件为ＯＤＳ柱，流动相甲醇：水＝７：３（ｖ／ｖ），紫外检测波长为２９０ｎｍ。在３ｈ左右测定浓度达峰值，其最高浓度分别为４．０１μｇ／ｍＬ和１１．４７μｇ／ｍＬ，五天左右下降为２．７３μｇ／ｍＬ和１．３２μｇ／ｍＬ附近。最小检出量为０．４ｎｇ／ｍＬ及０．７ｎｇ／ｍＬ。线性关系良好。丙硫咪唑砜和亚砜的回归相关系数分别为０．９９９４和０．９９９１。采用内标法测定回收率，平均为１００±１２％。     

稀土－二苯甲酰甲烷－三辛基氧化膦三元配合物的合成、表征、荧光特性及成膜性能

合成了三个稀土－二笨甲酰甲烷－三辛基氧化膦三元配合物Ｌｎ（ＤＢＭ）＿３·ＴＯＰＯ（Ｌｎ＝Ｙ、Ｅｕ、Ｅｒ）。用红外光谱、紫外光谱及差热—热重谱对其进行了表征，同时还研究了Ｅｕ（ＤＢＭ）＿３·Ｈ＿２Ｏ（Ａ）和Ｅｕ（ＤＢＭ）＿３·ＴＯＰＯ（Ｂ）在固态下及ＣＨＣｌ＿３溶液中的荧光光谱和荧光寿命，结果表明在ＣＨＣｌ＿３溶液中，Ｂ的荧光强度为Ａ的４８倍，其荧光寿命分别为（１４９±１０）μｓ和（８６±１０）μｓ。另外对这些化合物在空气／水界面的单分子膜行为也进行了研究。     

腹腔注射稀土化合物对小鼠肝脏抗氧化酶活性和脂质过氧化水平的…

成年小鼠每天腹腔注射０．２８ｍｍｏｌ／ｋｇ剂量的ＬａＣｌ３、Ｌａ－ＤＴＰＡ、ＴｂＣｌ３和Ｔｂ－ＤＴＰＡ生理盐水溶液，连续三天后与生理盐水对照组比较，ＬａＣｌ３使小鼠肝脏脂质过氧化（ＬＰＤ）水平升高，超氧歧化酶（ＳＯＤ）活性降低，而ＴｂＣｌ３的影响不明显；ＬａＣｌ３和ＴｂＣｌ３均显著降低谷胱甘肽过氧化酶（ＧＳＨ－Ｐｘ）活性。同样剂量Ｌａ－ＤＴＰＡ和Ｔｂ－ＤＴＰＡ对上述三项指标基本无影响。     

邻苯二胺-过氧化氢-辣根过氧化物酶酶联免疫示差脉冲伏安法测定人血清类风湿因子抗体

建立了邻苯二胺（ＯＰＤ）－Ｈ２Ｏ２－辣根过氧化物酶（ＨＲＰ）酶联示差脉冲伏安分析体系并用于测定人血清中类风湿因子（ＲＦ），ＨＲＰ催化Ｈ２Ｏ２氧化ＯＰＤ所形成酶催化产物在ｐＨ２．０磷酸盐－枸橼酸缓冲溶液中于－０．１８ Ｖ左右产生一灵敏示差脉冲伏安峰，ＲＦ浓度在１．２５～２０．０ Ｕ／ｍＬ之间与峰电流呈线性关系，应用此峰检测人血清ＲＦ的检测限低至 ０．２８Ｕ／ｍＬ。该法较相同条件下ＥＬＩＳＡ显色光度测定法的灵敏度增加５倍，且受干扰较少。     

功能聚间苯二胺膜用于免疫传感器分析

以电化学聚合法在石墨电极上获得聚间苯二胺膜（ＰＭＰＤ），并建立了快速、灵敏的膜质量检验方法：辣根过氧化物酶（ＨＲＰ）标记ＰＭＰＤ膜－邻苯二胺（ＯＰＤ）反应法，对聚合、活化等条件作了研究；进一步制成了检测乙肝表面抗原（ＨＢｓＡｇ）和检测鼠免疫蛋白（ＭＩｇＧ）的免疫电极，对血清样品作了检测．结果表明：２．５Ｖ电池电压下，于含０．１２ｍｏｌ／ＬＭＰＤ的１．２ｍｏｌ／ＬＨ２ＳＯ４中聚合２０ｍｉｎ，再以３０ｇ／Ｌ浓度的戊二醛活化４ｈ，所得ＨＲＰ标记电极及免疫电极重现性好；检测ＨＢ－ｓＡｇ和ＭＩｇＧ的线性范围分别为０．１～３．２ｍｇ／Ｌ及０．１～１０ｍｇ／Ｌ     

PBA光纤化学传感器在线监测家兔口服呋喃妥因的尿药浓度

芘丁酸光纤化学传感器（ＰＢＡ—ＦＯＣＳ）用于在线测定家兔口服呋喃妥因后排出尿液中的药物浓度。方法的检出限为１．３μｇ／ｍＬ，线性范围１～１００μｇ／ｍＬ，精密度（ＲＳＤ）１．５～３．５％，回收率在９５．０～１００％之间。４只雄性家兔的尿药浓度—时间曲线显示达峰时间为３．５ｈ，６ｈ累积尿药排出百分率为２１％。实验结果显示传感器、测定池和仪器系统设计合理。可实时、在线测定生物体液中的药物浓度并达到实用水平。     

THE RETENTION BEHAVIOR OF ARSENIC COMPOUNDS ON PRP-X100 COLUMN UNDER ALKALINE CONDITION

系统地研究了碱性条件下（ｐＨ８～１０．８）Ａｓ３＋，Ａｓ５＋，ＭＡ，ＤＭＡ和ＡＢ等砷化合物在ＰＲＰ－Ｘ１００阴离子交换柱上的保留行为。用火焰原子吸收光谱（ＦＡＡＳ）测定从ＨＰＬＣ分离的砷化合物，即通过一根１ｍ×０．２３ｍｍｉ．ｄ．不锈钢毛细管，将ＨＰＬＣ柱出口与ＦＡＡＳ的雾化器连接起来，采用乙炔／空气火焰，在１９３．７ｎｍ处测定。具体研究了两个流动相（２０ｍｍｏｌ／ＬＮＨ４ＨＣＯ３和２．５ｍｍｏｌ／Ｌ对－羟基苯甲酸－１．０ｍｍｏｌ／Ｌ苯甲酸水溶液），并系统研究了ｐＨ值和缓冲液浓度对上述５个砷化合物的保留时间的影响，发现对于２０ｍｍｏｌ／ＬＮＨ４ＨＣＯ３体系，在ｐＨ８．７时，ＡＢ，Ａｓ３＋，ＤＭＡ可以得到完全分离，通过梯度洗提（ｐＨ８．７到９．８，流速１．６５ｍＬ／ｍｉｎ），在１５ｍｉｎ内上述５个砷化合物可以得到良好分离；对于２．５ｍｍｏｌ／Ｌ对－羟基苯甲酸－１．０ｍｍｏｌ／Ｌ苯甲酸体系，在ｐＨ９．０及流速１．５ｍＬ／ｍｉｎ时，可以在１２ｍｉｎ内将上述５个砷化合物分离。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.