镧三元配合物的合成、热稳定性及生物活性

在甲醇介质中,用La(ClO4)3•nH2O与丙氨酸（CH3CHNH2COOH,简称Ala）及咪唑（C3H4N2,简称Im）或苯并咪唑(C7H6N2,简称BenIm)合成出两个新三元配合物La(Ala)3Im(ClO4)3•3H2O(简称La1)和La(Ala)3BenIm(ClO4)3•H2O(简称La2).对配合物进行了容量分析及元素分析，确定了其组成.通过IR、UV、XRD及TG-DTG、DSC进一步研究了配合物的配位行为及热稳定性.生物活性试验表明该类配合物对5种菌均具有不同程度的抑制作用.     

Synthesis and Crystal Structure of Two-dimensional Network Supramolecular Complex [Cu(dafo)_2(H_2O)_2](ClO_4)_2

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电感耦合等离子体质谱法测定人血浆中20种微量元素

建立了人血浆样品中微量元素的ICP-MS测定方法。分析了100名健康成人和50名健康儿童血浆样品的20种微量元素,给出了参考值范围。该方法检出限为0.0001~1.60μg/L;精密度(RSD)介于0.78%~4.27%;多数元素回收率在100%±10%之内。方法简便(正常人血浆经超纯水,硝酸,TritonX-100,正丁醇稀释后直接测定其中的微量元素),快速,样品用量少(血浆0.2mL),可作为人体内多种微量元素的监测方法,同时为人血浆中微量元素正常值范围的确定提供了参考依据。     

Synthesis of Nucleoside Derivatives Containing Benzophenoxazinone Moiety

Two new nucleoside derivatives containing benzophenoxazinone moiety were synthesized. Their luminescence spectra show that they have strong near infrared fluorescence.Our study provides a new method for direct introduction of near infrared fluorescent probe to bioactive molecules.     

A new method of UV-patternable hydrophobization of micro- and nanofluidic networks

This work reports a new method to hydrophobize glass-based micro- and nanofluidic networks. Conventional methods of hydrophobizing glass surfaces often create particulate debris causing clogging especially in shallow nanochannels or require skilful handling. Our novel method employs oxygen plasma, silicone oil and ultraviolet (UV) light. The contact angle of the modified bare glass surface can reach 100° whilst the inner channels after treatment facilitate stable and durable water-in-oil droplet generation. This modified surface was found to be stable for more than three weeks. The use of UV in principle enables in-channel hydrophobic patterning.     

Enzymatic Regioselective Synthesis of Vinyl Lactose Ester and Its Chemical Polymerization

Transesterification reaction of lactose with divinyladipate in pyridine catalyzed by an alkaline protease from Bacillus subtilis at 50℃ for 3 days gave 6′-O-vinyladipoyl-lactose (yield 35%).Poly (6′-O-vinyladipoyl-lactose) with Mn=21,200,Mw=32,900,Mw/Mn=1.56 could be obtained by chemical polymerization. Poly(vinyl alcohol) containing lactose branch was biodegradable. After 6 days in aqueous buffer(PH7), this alkaline protease could degrade the polymer to an Mn of ca. 2100,Mw/Mn=2.56.     

液相色谱-串联质谱法同时测定三七中508种农药残留

采用液相色谱-串联质谱(LC-MS/MS)建立了可在20 min内快速测定三七中508种农药残留的方法。样品经改良的QuEChERS方法提取,分散固相萃取法(d-SPE)净化后,在多反应监测(MRM)模式下进行LC-MS/MS分析,内标法定量。在优化实验条件下,508种农药均在0.005～0.4 mg/L范围内线性关系良好,方法检出限(LOD)为0.005～0.1 mg/kg;在100μg/kg加标水平下,除8种农药外,其余500种农药的回收率均在50.2%～117%之间,且相对标准偏差(RSD)均不大于15%;其中有468种农药的回收率为70%～120%。该方法样品前处理简单快速,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于三七中508种农药残留的快速筛查。     

LaCl3提高菠菜光系统Ⅱ活性的作用机制

The effect of LaCl3 on the K3Fe(CN)6 (FeCy) reduction rate and the oxygen-evolving rate of PSU particles of spinach, and the spectral characterization of the D1/D2/Cytb559 of a PSII reaction center complex consisting of three polypeptides from spinach were studied. The experimental results showed that LaCl3 could significantly accelerate the transformation from light energy to electric energy, the electron transport, water photolysis and oxygen evolution of PSII of spinach, which was related to the spectral characterization of the D1/D2/Cytb559 complex.Soret band and Q band of Chl-a of UV-vis spectrum of D1/D2/Cytb559 complex were blue shifted, and the fluorescence emission peak was blue shifted in LaCl3 treated spinach compared with that in the control. The EXAFS (extended X-ray absorption fine structure spectroscopy) revealed that La^3 was coordinated with 8 nitrogen or oxygen atoms in the first coordination shell with La-N or La-O bond length of 0.254 nm, and with 6 nitrogen or oxygen atoms in the second coordination shell with La-N or La-O bond length of 0.321 nm in the D1/D2/Cytb559 complex. The CD suggested that the secondary structure of D1/D2/Cytb559 complex have been litfie affected by the treatment of LaCl3.     

Derivatization-independent cholesterol analysis in crude lipid extracts by liquid chromatography/mass spectrometry: applications to a rabbit model for atherosclerosis

Direct measurement of various sterols in crude lipid extracts in a single experiment from limited biological samples is challenging. Current mass spectrometry (MS) based approaches usually require chemical derivatization before subjecting to MS analysis. Here, we present a derivatization-independent method for analyzing various sterols, including cholesterol and its congeners, using liquid chromatography and atmospheric pressure chemical ionization mass spectrometry. Based on the specific tandem mass spectrometry pattern of cholesterol, multiple reaction monitoring (MRM) transitions were used to quantify free cholesterol and its fatty acyl esters. Several cholesterol oxidation products could also be measured using the upfront liquid chromatography separation and specific MRM transitions. The method was validated alongside established enzymatic assays in measuring total cholesterol. As a proof of concept, we analyzed plasma sterols in rabbits administrated with a high cholesterol diet (HCD) which is a classical atherosclerotic model. Free cholesterol, cholesterol esters, 7-hydroxycholesterol, and 7-ketocholesterol were elevated in plasma of rabbits on HCD. This method could also serve as an excellent tool for quantitative analysis of other sterols such as ergosterol and sitosterol in other organisms beside mammalian. In Saccharomyces cerevisiae, our results indicated dramatic increases of the ratio of ergosterol esters to free ergosterol in both yeh2Δ and tgl1Δ cells, which are consistent with the function of the respective enzymes.     

Supramolecular Architectures of Four New Transition Metal Complexes with 3‐[4‐(Carboxymethoxy)phenyl]propanoic Acid and N‐[4‐(Carboxymethoxy)phenyl]iminodiacetic Acid

Four new transition metal complexes: [Cu(Hcppa)₂(H₂O)₂] ( 1 ), [Co₂(cppa)₂(H₂O)₁₀] ( 2 ), [Co₃(cpia)₂(H₂O)₈] · 2H₂O ( 3 ) and [Ni₃(cpia)₂(H₂O)₁₂] · 6H₂O ( 4 ) {H₂cppa = 3‐(4‐(carboxymethoxy)phenyl]propanoic acid; H₃cpia = N‐[4‐(carboxymethoxy)phenyl]iminodiacetic acid} were synthesized and characterized. Complexes 1 and 2 show mononuclear structures, complexes 3 and 4 exhibit dinuclear structures. All complexes extend to 3D supramolecular networks through hydrogen bonds, of which complexes 3 and 4 display microporous structures. In complexes 2 – 4 the water clusters are trapped by the cooperative association of coordinate interactions as well as hydrogen bonds, forming different 1D metal‐water chain structures. Thermal stabilities of complexes 1 – 4 were discussed.