Hybrid NAA method for assessment of the levels of organic halogen compounds in the atmosphere in China

Abstract Passive air samplers (polyurethane foam disks) were deployed at 25 urban sites and 66 rural sites over the period of July to October 2005, partly between October 2005 and January 2006 for about 120 days across China, and analyzed for extractable organo-chlorine /-bromine /-iodine (EOCl/EOBr/EOI) and polychlorinated biphenyls (PCBs) using hybrid neutron activation analysis (NAA) combined with gas chromatographymass spectrometry (GC-MS). The average concentration of EOCl, EOBr, EOI and ΣPCBs among all the sites were 173.7, 3.5, 1.0 and 0.74 ng/d, respectively. Higher values of EOCl/Br/I and PCBs were detected in the areas of high usage and high emission, which were linked to relatively high-income areas in China, while lower in the west ill-developed region of China, which indicated that these pollutants mainly came from industrial pollution. Higher EOCl contents in traffic areas stated that the exhaust emission from vehicle was another main source of organochlorines in the air. The relative proportions of the known organochlorines (84 PCB congeners) to total EOCl were 0.02–3.0%, which implied that most of EOCl measured in air were unknown.     

电感耦合等离子体质谱间接法测定蛋白质含量

尺寸排阻色谱分离牛血清白蛋白(BSA),超氧化物歧化酶(SOD)和金属硫蛋白(MT)等3种标准蛋白的混合物后,在线使用电感耦合等离子体质谱测定这三种蛋白中的S,并根据每种蛋白质含有的S原子数,计算出3种蛋白质的相对含量。尺寸排阻色谱的流动相为0.1mol/LTris-HAc。向电感耦合等离子体质谱的六级杆加入反应气O2,使之与S反应生成SO ,间接测定32S16O 而避开直接测量32S时存在的严重干扰。测量结果与天平称量所得结果一致。方法的精密度好,每个蛋白质峰面积的RSD<3%(n=3)。BSA、SOD和MT的检出限分别为14、52和27pmol。     

Characterization of constituents in Stellera chamaejasme L. by rapid-resolution liquid chromatography-diode array detection and electrospray ionization time-of-flight mass spectrometry

A reliable and rapid method based on rapid-resolution liquid chromatography-diode array detection (RRLC-DAD) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) has been developed for the isolation and characterization of multiple constituents in the root of Stellera chamaejasme L., which was extracted by sonication with methanol in an optimized procedure. Separation of the multiple constituents was achieved on an Agilent Zorbax XDB-C18 (50x3.0 mm i.d.; 1.8 microm) column using a gradient elution at a flow rate of 0.4 mL/min. The detection wavelength was 210 nm. Mass spectra were acquired in both positive and negative modes. A formula database of the known chemical constituents in the root of Stellera chamaejasme L. was established by an Agilent software. Twenty-two obvious peaks appeared in the total ion chromatogram and nine of them were characterized by TOF/MS. The RRLC-DAD and ESI-TOF/MS method with ultrasonic extraction would be useful for rapid and effective characterization of chemical constituents in the root of Stellera chamaejasme L.     

Synthesis and application of a new copper(II) complex containing oflx and leof

Two new copper(II) complexes of [Cu(Ofloxacin)(phen)(H₂O)] · (NO₃) · 2H₂O and [Cu(Levofloxacin)(phen)(H₂O)] · (NO₃) · 2H₂O were obtained and their structures were studies. Both ligands and complexes were assayed against gram-positive and gram-negative bacteria by the in vitro doubling dilutions method. The inhibitory effect of the ligands and complexes on the leukemia HL-60 cell line were measured with the MTT assay method and the liver cancer HePG-2 cell line measured by the SRB method. The results indicated that the complexes have stronger inhibitory effect on HL-60 than on HePG-2. The complex [Cu(Levofloxacin)(phen)(H₂O)] · (NO₃) · 2H₂O (I) has stronger effect on HL-60 than the complex (Cu(Ofloxacin)(phen)(H₂O)] · (NO₃) · 2H₂O (II). The text was submitted by the authors in English.     

Simultaneous Determination of the Active Ingredients in Abelmoschus manihot (L.) Medicus by CZE

A capillary zone electrophoretic method has been developed for the quantitative analysis of four active compounds, quercetin-3-O-robinobioside (LXY3), hyperin (LXY4), isoquercetin (LXY5) and myricetin (LXY7) in A. manihot (L.) Medicus with UV detection at 254 nm. The capillary temperature was kept constant at 25 °C. The effects of buffer composition, pH, and concentration and running voltage on migration were studied systematically. Optimum separation was achieved with 20 mmol L^?1 Borax–NaOH buffer (pH 9.50) at 25 °C and 25 kV. Regression equations revealed good linear relationship between the peak area of each compound and its concentration. All the correlation coefficients were higher than 0.9990. The relative standard deviations of migration time and the peak area were <0.53% and 5.34% (inter-day), and <0.56% and 3.81% (intra-day). The contents of the four compounds in A. manihot (L.) Medicus were successfully determined with satisfactory repeatability and recovery.     

气相色谱/气质联用分析食品及环境基质中特丁硫磷残留量

建立在食品及环境样品中特丁硫磷残留量的气相色谱检测及气质联用确证法。样品采用乙酸乙酯提取、活性炭-酸性氧化铝复合小柱净化,丙酮-正己烷混合溶液（体积比为1：9）洗脱,样液浓缩后经GC—FPD检测．外标法定量,GC—MS定性。GC—FPD法分析时,特丁硫磷在不同样品、不同水平的加标回收率为74．5％～103．3％．RSD为2．1％～11．7％（n=5）,方法的检出限为0．001mg／kg.气质联用法确证时,特丁硫磷的SIM离子为186、231（Q,100）、288.     

A New Enzyme Immobilization Technique Based on Thionine‐Bovine Serum Albumin Conjugate and Gold Colloidal Nanoparticles for Reagentless Amperometric Biosensor Applications

A novel enzyme immobilization technique based on thionine‐bovine serum albumin conjugate (Th‐BSA) and gold colloidal nanoparticles (nano‐Au) was developed. Thionine was covalently bound onto the BSA film with glutaraldehyde(GA) as cross‐linker to achieve Th‐BSA conjugate. The free amino groups of thionine were then used to attach nano‐Au for the immobilization of horseradish peroxidase (HRP). Such nano‐Au/Th‐BSA matrix shows a favorable microenvironment for retaining the native activity of the immobilized HRP and thionine immobilized in this way can effectively shuttle electrons between the electrode and the enzyme. The proposed biosensor displays excellent catalytic activity and rapid response for H₂O₂. The linear range for the determination of H₂O₂ is from 4.9×10^?7 to 1.6×10^?3 M with a detection limit of 2.1×10^?7 M at 3σ and a Michaelies‐Menten constant K value of 0.023 mM.     

Temperature-Triggered Structural Dynamics of Non-Coordinating Guest Moieties in a Fluorescent Actinide Polyrotaxane Framework

We present here the synthesis of a novel fluorescent actinide polyrotaxane compound URCP1 through the utilization of an end-cutting pseudorotaxane precursor with only the cucurbit[6]uril (CB[6]) macrocyclic components acting as linking struts. The non-coordinating guest motif in the obtained polyrotaxane, with increased freedom and structural flexibility, can display intriguing temperature-triggered conformational variations inside the cavity of CB[6], which was clearly evidenced by crystallographic snapshots at different temperatures. Notably, this observation of temperature-triggered structural dynamics in URCP1 represents the first report of actinide polyrotaxane with such feature in solid-state. Moreover, URCP1 has a high photoluminescence quantum yield (PLQY) of 49.8 %, comparable to other luminescent uranyl compounds, and can work as a fluorescent probe to selectively detect Fe³⁺ over other eight competing cations in aqueous solution, with the limit of detection being as low as 4.4×10⁻³ ppm.     

Electrochemical Behaviour and Chemical Species of Sm(II) in AlCl3-NaCl with Different Lewis Acidity

AlCl₃-NaCl was utilized as an electrolyte in this work due to its low melting point and Lewis acidity, in which samarium exists in two oxidation states, Sm(III) and Sm(II), resulting in unique electrochemical behaviours. Sm metal dissolves in AlCl₃-NaCl melt to form SmCl₂, which is verified by electrochemical and spectroscopic techniques. As the Lewis acidity of the melt increases, the diffusion coefficient of Sm(II) gradually increases, and the activation energy of diffusion decreases. Moreover, an additional co-reduction peak of Sm³⁺ and AlCl₄⁻ is observed to be more positive than that of Al(0)/Al(III) in Lewis basic melt, which may be tightly correlated with the variation of Sm(II) coordination in AlCl₃-NaCl melt and ligand variation from Cl⁻ to AlCl₄⁻ and Al₂Cl₇⁻ as the Lewis acidity of the AlCl₃-NaCl melt increases, according to the in situ electronic absorption spectra of Sm in this melt.