方胺功能化荧光金属-有机框架材料的制备及对组氨酸的识别研究

以方胺功能化配体5,5′-[(3,4-二氧环丁-1-烯-1,2-二基)二(氮烷二基)]二间苯二甲酸(H_(4)L)和六水合硝酸钴为原料,在碱性条件下通过水热反应制备了一种方胺功能化的金属-有机框架材料(Co-L).X射线单晶衍射结果显示,该材料是由一维链通过CH…π和氢键相互作用形成的三维网络结构,在b轴和c轴方向分别存在窗口直径为0.52和0.63 nm的一维孔道.荧光测试结果表明,Co-L可在20种天然氨基酸中高选择性地检测组氨酸,并对其检测机理进行了研究.

一些方酰磺酰亚胺类化合物的合成

一些方酰磺酰亚胺类化合物的合成李聚才周海兵陈益钊（化学系）在方酸化学中，未见方酰基和磺酰基的酰亚胺类化合物的报道，为此我们开展了相关的初步研究．要制备酰亚胺类化合物，通常用胺或酰胺与活性更高的酸酐［１，２］反应来制备．试图用苯磺酰胺与方酸直接反应以获...

纳米聚多巴胺六方氮化硼–二氧化硅/环氧树脂涂层对水泥砂浆抗碳化能力的影响

为了获得具有良好分散性、填充性和阻隔性的纳米材料,同时将其作为填料以提升环氧树脂涂层对水泥砂浆试件的防护能力,本文制备了纳米聚多巴胺六方氮化硼–二氧化硅(PDABN-fSiO_(2))/环氧树脂涂层,涂覆于水泥砂浆试件表面,研究涂层对试件的防护效果。首先,利用盐酸多巴胺(DA)自聚合形成的聚多巴胺(PDA)与偶联剂(KH550),分别修饰纳米六方氮化硼(hBN)与纳米二氧化硅(SiO_(2)),获得纳米聚多巴胺六方氮化硼(PDABN)与功能化的SiO_(2)(fSiO_(2));其次,经聚合以制备纳米PDABN-fSiO_(2);最后,将其作为填料改性环氧树脂,并涂覆于水泥砂浆表面。通过FTIR、SEM-EDS和XPS等微观表征,观察并研究了纳米材料的微观特征;开展了碳化试验和涂层透气性试验,分析了纳米PDABN-fSiO_(2)对环氧树脂涂层的改性效果。结果表明:制备的纳米PDABN-fSiO_(2)具有“片层+颗粒”特殊结构,且在涂层中具有良好的分散性,可有效减缓其涂层中CO_(2)的渗透;同无填料涂层相比,涂覆有纳米PDABN-fSiO_(2)/环氧树脂涂层的水泥砂浆试件,在碳化7天、14天和28天时的碳化深度分别下降了68.7%、72.9%和64.8%,其涂层在48 h的透气性降低了34.7%。因此,纳米PDABN-fSiO_(2)掺入环氧树脂涂层后,明显地提高了涂层水泥砂浆试件的抗碳化能力,并降低了环氧树脂涂层的透气性。

基于异斯特维醇的新型伯胺-方酰胺催化的高对映选择性Michael加成反应

新型双功能伯胺-方酰胺能有效催化醛与马来酰亚胺的不对称Michael加成反应.应用此法,可简便地制备一系列取代的琥珀酰亚胺衍生物,并能以高产率(高达98%)和优秀的对映选择性(高达>99%ee)分别得到相应加成产物的两个异构体.

2-[(1’S,2’R)-(2’-羟基-1’,2’-二苯基乙基)氨基]-3,4-二酮环丁烯硫醇钠的表征与应用

针对2-[(1’S,2’R)-(2’-羟基-1’,2’-二苯基乙基)氨基]-3,4-二酮环丁烯硫醇钠的结构,通过元素分析,红外光谱及核磁共振进行了表征,并考察了它与常见金属离子的作用。实验表明,该化合物是一个优良的手性配体。

Renaldopaminergic system:Pathophysiological implications andclinical perspectives

Fluid homeostasis, blood pressure and redox balance in the kidney are regulated by an intricate interaction between local and systemic anti-natriuretic and natriuretic systems. Intrarenal dopamine plays a central role on this interactive network. By activating specifc receptors, dopamine promotes sodium excretion and stimulates anti-oxidant and anti-inflammatory pathways. Different pathological scenarios where renal sodium excretion is dysregulated, as in nephrotic syndrome, hypertension and renal infammation, can be associated with impaired action of renal dopamine including alteration in biosynthesis, dopamine receptor expression and signal transduction. Given its properties on the regulation of renal blood fow and sodium excretion, exogenous dopamine has been postulated as a potential therapeutic strategy to preventrenal failure in critically ill patients. The aim of this review is to update and discuss on the most recent findings about renal dopaminergic system and its role in several diseases involving the kidneys and the potential use of dopamine as a nephroprotective agent.

Selective flotation of smithsonite, quartz and calcite using alkyl diamine ether as collector

The flotation separation of smithsonite from calcite and quartz using a alkyl diamine ether(GE-609)as the collector was investigated through micro-flotation experiments and the real ore flotation experiments.The results show that GE-609exhibits good collecting capability to three minerals without selectivity.The presence of sodium sulfide enhances the flotation of smithsonite and calcite while inhibits quartz.Moreover,both sodium silicate and sodium hexametaphosphate exhibit good selective inhibition to calcite.The real ore test results show that a zinc concentrate containing23.51%Zn with the recovery of71.02%is obtained in the closed-circuit test.To understand the adsorption of GE-609on smithsonite surface,zeta potential measurement and FTIR analysis were carried out,and the results indicate that the collector GE-609can adsorb on smithsonite surface through both electrostatic adsorption and chemical adsorption,and the presence of sodium sulfide enhances the adsorption of GE-609.

Severe cyclophosphamide-related hyponatremia in a patient with acute glomerulonephritis

Cyclophosphamide is frequently used to treat cancer,autoimmune and renal diseases,such as rapidly progressive glomerulonephritis.Its side effects are well-known,including bone marrow depression,infections,alopecia,sterility,bladder malignancy and hemorrhagic cystitis.Moreover,in some cases cyclophosphamide use has been related to the onset of hyponatremia,by development of a syndrome of inappropriate antidiuresis.Indeed,severe hyponatremia has been previously reported in patients treated with high-dose or moderate-dose of intravenous cyclophosphamide,while only few cases have been reported in patients treated with low dose.Here,we discuss a case of a syndrome of inappropriate antidiuresis followed to a single low-dose of intravenous cyclophosphamide in a patient with a histological diagnosis of acute glomerulonephritis,presenting as acute kidney injury.After cyclophosphamide administration(500 mg IV),while renal function gradually improved,the patient developed confusion and headache.Laboratory examinations showed serum sodium concentration dropped to 122 mmol per liter associated with an elevated urinary osmolality of 199 mO sm/kg,while common causes of acute hyponatremia were excluded.He was successfully treated with water restriction and hypertonic saline solution infusion with the resolution of the electrolyte disorder.This case,together with the previous ones already reported,highlights that electrolyte profile should be strictly monitored in patients undergoing cyclophosphamide therapy in order to early recognize the potentially lifethreatening complications of acute water retention.

Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-（3-nitro-4-methoxyphenyl） Acetamide

Deactivation of Pd/C catalyst often occurs in liquid hydrogenation using industrial materials. For in-stance, the Pd/C catalyst is deactivated severely in the hydrogenation of N-(3-nitro-4-methoxyphenyl) acetamide. In this study, the chemisorption of sulfur on the surface of deactivated Pd/C was detected by energy dispersive spec-trometer and X-ray photoelectron spectroscopy. Sulfur compounds poison the Pd/C catalyst and increase the forma-tion of azo deposit, reducing the activity of catalyst. We report a mild method to regenerate the Pd/C catalyst: wash the deposit by N,N-dimethylformamide and oxidize the chemisorbed sulfur by hot air. The regenerated Pd/C cata-lyst can be reused at least ten runs with stable activity.

Treatment of bauxite residue dust pollution by improving structural stability via application of synthetic and natural polymers

The residue drying area(RDA)is the major source of fugitive red sand(RS)dust emissions in the bauxite mining industry and causes serious environmental and safety detriments.Polymer stabilizer(PS)is one of the promising non-traditional stabilizers to mitigate such issues.This research investigated the unconfined compressive strength(UCS)of RS using synthetic polymer stabilizer(SPS)and natural polymer stabilizer(NPS),and to determine the optimum application concentration and mixing ratio of the PAM and Guar gum mixture.Results illustrated that PAM apparently outperform Guar gum in stabilizing sand particles.The mixture of PAM and Guar gum is more effective than individual use.The optimum polymer concentration and the mixing ratio are 0.94 wt.%and 0.6(PAM:total(PAM+Guar gum)),respectively.A rigorous regression model was developed to predict the UCS value based on application concentration and mixing ratio for the purpose of cost and time efficiency.

Ship-in-bottle synthesis of NaY zeolite encapsulated Cosalen complex and its catalytic performance for cyclohexane oxidation

N, N＇-bis （salicylidene） ethylenediiminocobalt （Cosalen） was encapsulated into microporous NaY zeolite via the technique of ＂ship-in-bottle＂. The encapsulated complex （Cosalen-NaY） was characterized by Fourier-transform infrared spectrum, ultraviolet-visible spectrum, Brunaner-Emmett-Teller surface areas, X-ray diffraction, thermogravimetry-differential thermal analysis and scanning electron microscope. The reaction of cyclohexane oxidation using oxygen was chosen to investigate the catalytic performance of Cosalen-NaY, and the effects of oxygen pressure, temperature and reaction time were also studied. The results show that Cosalen complex is encapsulated into the supercage of the zeolite and the structure of NaY zeolite remains integrity and the thermal stability of Cosalen is greatly enhanced after encapsulation. Cosalen-NaY shows the better activity in the oxidation of cyclohexane without reductant and solvent. The conversion of cyclohexane is up to 13.4% at 150 ℃ for 3 h under oxygen pressure of 0.85 MPa, with the higher total selectivity to cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide （CHHP） and acid （79.2%） than the neat complex （55.5%）. NaY zeolite cartier maybe contributes to the results. There is no obvious induction period to initiate the reaction; furthermore, the amount of CHHP among the products is small, which indicates that the Cosalen-NaY has the strong ability to accelerate the decomposition of CHHP. Recycling tests show that the hybrid material can be used repeatedly with a negligible loss of active sites.

A Chinese Compound Prescription Ding Xin Recipe Combined with Amiodarone for Treating Premature Ventricular Complexes: A Randomized, Double-Blind, Multicenter, Placebo-Controlled Trial

Objective To evaluate the efficacy and safety of Ding Xin Recipe(DXR)combined with amiodarone in patients with PVCs.Methods A total of360patients with PVCs across7centers in China were randomly assigned in a1:1:1ratio to receive up to8weeks of amiodarone combined with DXR placebo(amiodarone group),DXR combined with amiodarone placebo(DXR group),or DXR combined with amiodarone(DCA group)from July2012to December2013.Randomization was conducted according to a centralized randomization schedule prepared by an independent steering committee.Staff and patients at all sites were masked to treatment allocation.All patients received best-evidence advice.The primary outcome was the efficacy for treating PVCs,with efficacy assessed by the reduction of premature ventricular contractions.Other outcome measures included PVCs-related symptom scores.All data were analyzed by intention to treat.Results The efficacy for treating PVCs in the DCA group(90.7%)significantly increased compared with that in the amiodarone group(72.3%)and the DXR group(73.9%).The frequency,the degree,and the duration per week of heart palpitations,chest tightness,shortness of breath and fatigue improved significantly in the DCA group in comparison with the amiodarone group and the DXR group(P<0.05),while no significant difference was observed in the improvement of insomnia among the three groups(P>0.05).With regard to laboratory parameters for safety,there were no clinically relevant changes in the three groups.Conclusion The present study demonstrates that DXR combined with amiodarone is significantly more effective than DXR or amiodarone alone for treating PVCs.

Characteristics and therapeutic efficacy of sulfasalazine in patients with mildly and moderately active ulcerative colitis

AIM: To investigate the characteristics and short-term efficacy of sulfasalazine (SASP) in patients with mildly and moderately active ulcerative colitis (UC).METHODS: Two hundred and twenty-eight patients with mildly and moderately active UC were recruited, 106patients in 1993-1995, and 122 patients in 2000-2002,they were assigned as the 1990s group (n = 106) and the 2000s group (n = 122), prospectively. The general characteristics, clinical manifestations, colonoscopic and histological data were compared between the two groups.The short-term efficacy and safety of SASP 3 g per d were evaluated.RESULTS: Between 2000s and 1990s groups, the gender ratio of men to women was 1:1.18 and 1:1.04, 57.4%and 50.9% of the patients were between 30 and 49 years old. The gender ratio and age of UC patients were not significantly different. The total course of 50.0% and 37.1% of UC patients was less than 1 year (P＜0.05), 10.6% and 31.2% of the cases had a duration of more than 5 years (P＜0.05) in 2000s and 1990s groups, respectively. The most common clinical type was first episode in 2000s group and chronic relapse in 1990s group. The patients showed a higher frequency of abdominal pain and tenderness in 1990s group than in 2000s group. Erosions were found in 84.4% and 67.9% of patients in 2000s and 1990s groups (P＜0.05). Rough and granular mucosa (67.9%vs43.4%, P＜0.05)and polyps (47.2% vs 32.8%, P＜0.05)were identified in 1990s group more than in 2000s group.There were no significant differences in clinical, colonoscopic and histological classifications. After SASP (1 g thrice per d) treatment for 6 wk, the clinical, colonoscopic and histological remission rates were 71.8%, 21.8% and 16.4%,respectively. In 79 patients with clinical remission, 58.2%and 67.1% remained grade 1 in colonoscopic and histological findings, respectively. The overall effects in first episode type (complete remission in 10, 18.9%, partial remission in 28, 52.8%, and improvement in 9, 17.0%) were better than in chronic relapse type (complete remission in 3,7.5%; partial remission in 16, 40.0%; and improvement in 15, 37.5%) and chronic persistent type (complete remission in 1, 5.9%; partial remission in 6, 35.3%; and improvement in 6, 35.3%) respectively (P＜0.05). In 110patients treated with SASP, 18 patients (16.4%) had adverse reactions. Except for two cases of urticaria and one case of WBC decrease, none of the patients had to stop the treatment because of severe adverse reactions.CONCLUSION: Patients with mildly and moderately active UC in 2000s group had a shorter disease course, milder clinical manifestations, more first episode type and higher frequency of acute mucosal lesions in colonoscopy than in 1990s group. The patients in 1990s group had higher proportion of chronic relapse type and chronic mucosal change in colonoscopy than in 2000s group. The shortterm efficacy of SASP could be mainly remission of clinical manifestations. But more than half of the patients still had light inflammation in colonoscopy and histology. The overall effects of SASP in first episode type were better than those in other types. SASP was a safe and effective drug to treat mildly and moderately active UC.

SYNTHESIS AND CHARACTERIZATION OF HETEROAROMATIC POLYMERS CONTAINING PYRIDINE MOIETIES

The progress on the molecular design, synthesis and characterizations of some kinds of pyridine-containing heteroaromatic polymers in main chain were reviewed in this paper, they would include polyimides （Pls）, polypyrrolones （PPYs）, poly（pyrrolane-imide）s （PPIs）, and poly（pyrrolane-benzimidazone）s （PPBs） containing pyridine moieties. The pyridine-cantaining polymers reported all exhibit good processability, excellent thermal properties and mechanical properties. However, the contribution of pyridine ring to polymers properties is still need to research further, the heteroaromatic polymers containing pyridine moieties have focused by more and more researchers.

Significance of Biogenic Amines in Foods and Their Reduction Methods

The term ＂biogenic amines＂ defines decarboxylation products such as histamine, putrescine, serotonin, tyramine, phenylethylamine, tryptamine and also aliphatic polyamines. They can be detected in both raw and processed foods. In the recent years, there is a great interest in biogenic amines as they are associated with quality, safety and freshness of some foods, particularly fermented foods. The presence of biogenic amines in foods can also be used as an indicator of hygienic quality. Biogenic amines also cause health hazards due to their toxic effects especially in sensitive individuals. It is therefore important to control and reduce the biogenic amines. The reduction can be brought about by the use of high pressure, irradiation, packaging, additives, starter cultures and by reduction of decarboxylase activity and temperature. This review summarizes the significance, function, occurrence and formation of biogenic amines in different foods and their reduction by different methods.

Square Wave Voltammetric Behavior of N,N-DiethyI-P-Nitroso Aniline an Indirect Method for Determination of Chlorpheniramin Maleate, Application of Pharmaceutical Formulations

The electrochemical behavior of N,N-diethyl-p-nitroso aniline was carried out using SWV （square wave voltammetric） at HMDE. A well defined reduction peak was observed at （-0.214） volt versus the reference electrode （Ag/AgC1/sat. KCI）, calibration curve was constructed in phosphate buffer （pH = 7.0）, the relationship is linear within the concentration range 1.283 × 10.5 M - 3.66 × 10.5 M with the correlation （R = 0.9923）. The serial addition ofCPM （chlorpheniramine maleate） leads to the decrease in the reduction current peak （Ip）, quantitatively, the plot of Alp （Ip - Ip） where, Ip： Peak current of N, N-diethyl-p-nitroso aniline alone, lp： peak current of N,N-diethyl-p-nitroso aniline in the presence of CPM, versus concentration is linear within the concentration range 0.984 × 10-6 M - 9.756 × 10-6 M, the correlation coefficient was 0.9954. The method was successfully applied to determine CPM in different types of pharmaceutical formulations, and compared with standard method from British Pharmacopeia [1].

Optimization strategies for separation of sulfadiazines using Box-Behnken design by liquid chromatography and capillary electrophoresis

Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.

Preparation and characterization of poly(amic acid)-stabilized silver nanoparticles

Stable and monodispersed silver nanoparticles were produced through a mild,convenient,one-pot method based on the reduction of silver nitrate in the presence of poly(amic acid) (PAA) as a stabilizer.The surface plasma band transition was monitored along with time in the reaction mixture for three sets of experiments by ultraviolet-visible spectroscopy.Analysis of the data with the Avrami equation yielded n exponent with values between 0.5 and 1.5,demonstrating three-dimensional heterogeneous nucleation and diffusion-controlled growth,accompanied by soft impingement effect.XRD and TEM analyses show a softly agglomerated polycrystalline state and a nearly spherical morphology (<50 nm) of nanoparticles.The FT-IR result indicates that the PAA molecular structure could be hardly influenced by the formation of nanoparticles.