Preparation of Titania Monolith Column and Application in Determination of Benzoic Acid by HILIC

The titania monolith column has been synthesized through a template-free sol–gel route, and a simple and reliable method for the determination of benzoic acid by hydrophilic interaction liquid chromatography using the prepared titania monolith has been developed. The influences of acetonitrile, acetate buffer and buffer pH on the retention of benzoic acid were investigated. Benzoic acid in carbonated drinks and fruit beverages samples were determined within 5 min and quantitative analysis was carried out by external standard method with a correlation coefficient (R ²) of 0.9984. The relative standard deviation was 0.91 % and the recovery ranged from 92.5 to 101.3 %. The proposed method is suitable for the analysis of benzoic acid in beverage samples.

     

Metabolite Identification of Myricetin in Rats Using HPLC Coupled with ESI-MS

Myricetin, a naturally occurring flavonol, shows multifarious pharmacological activities, e.g., antidiabetic, antioxidant, anti-inflammatory, antitumor, and liver protection effects. In order to obtain an understanding of the myricetin’s metabolism in vivo, a rapid and sensitive method by high-performance liquid chromatography coupled with electrospray-ionization mass spectrometry (HPLC-MSⁿ) techniques was employed to investigate the biotransformation in rats after oral administration of myricetin. Recognition and structural exposition of the metabolites were operated by comparing the changes in molecular mass (ΔM) and MSⁿ spectra with the parent drug. As a result, the parent compound and seven metabolites were found in rat plasma, urine, and feces. In addition, besides 3,5-dihydroxyphenylacetic acid (M1) and 3,4,5-trihydroxyphenylacetic acid (M2), five other compounds were first discovered in the metabolite research of myricetin. These results indicated that, besides ring-fission, there were methylate (M3, M4, M5) and glucuronide (M6, M7) biotransformations of myricetin occurring in vivo.

     

不对称三苯胺-锌酞菁的合成及性能研究

以对氨基酚、对硝基氯苯、8-羟基喹啉、4-硝基邻苯二甲腈以及醋酸锌为主要原料,合成了不对称2(3)-[二(对硝基苯基)氨基苯氧基]-9(10),16(17),23(24)-三(8-喹啉氧)锌酞菁(TQPc).用核磁、红外、元素分析等表征TQPc以及前驱化合物结构,TQPc的电子吸收光谱表现出了强烈的π-π*跃迁现象.利用紫外光谱研究了其N,N-二甲基甲酰胺(DMF)和CH2Cl2溶液的吸收光谱性质,结果表明在DMF中主要以单体的形式存在,浓度在0.223×10-5～2.587×10-5mol/L时,TQPc在CH2Cl2溶液中有二聚体的存在,经计算得到平衡常数为0.24×105L/mol.用循环伏安法研究了TQPc的氧化还原行为,结合差分伏安数据计算了能级结构,LUMO(-1.04 V vs SCE)和HOMO(0.78 V vs SCE)与纳米TiO2导带能级匹配,可作为性能较好的电荷传输材料用于染料敏化太阳能电池.     

Kinetics investigation on the combustion of waste capsicum stalks in Western China using thermogravimetric analysis

The combustion kinetics of waste capsicum stalk (WCS) in Western China is investigated through thermogravimetric analysis compared with sawdust and coal, and co-combustion of WCS with coal is also investigated. Results show that the ignition characteristics of WCS is better than that of sawdust and coal, and the activation energy E of WCS-volatile combustion and WCS-char combustion are 78.55?kJ?mol^?1 and 44.59?kJ?mol^?1. However, integrating the characteristics of ignition and burnout, the combustion characteristic factor (S _N) of WCS is lower than that of sawdust. With the increasing in the heating rate, the ignition of WCS is delayed. Oxygen concentration $ C_{{{\text{O}}_{2} }} $ affects E and k ₀ of volatile combustion largely under rich-oxygen condition, when $ C_{{{\text{O}}_{2} }} $ increases from 0.2 to 0.8, E has increased threefold and k ₀ also intensively increases from 10⁶ to 10¹³?C10²². Oppositely, effect of $ C_{{{\text{O}}_{2} }} $ on the E and k ₀ of char combustion is little, and there is an exponential relationship $ S_{\text{N}} = 7. 1 2 8 \times 10^{ - 9} \times { \exp }(C_{{{\text{O}}_{2} }} /0. 3 6 8) - 6. 1 2 6 \times 10^{ - 9} $ between S _N and $ C_{{{\text{O}}_{2} }} $ . For the tests of co-combustion, all the experimental and weighted-average curves coincide well, and there is no remarkable synergistic effect. With the increase of mixing ratio that WCS added, E and k ₀ of volatile combustion increase, but correspondingly E and k ₀ of char combustion decrease.     

Synthesis, structural characterization and electrochemical studies of nickel(II), copper(II) and cobalt(III) complexes of some ONS donor ligands derived from thiosemicarbazide and S-alkyl/aryl dithiocarbazates

Four tridentate ONS ligands, namely 2-hydroxyacetophenonethiosemicarbazone (H₂L¹), the 2-hydroxyacetophenone Schiff base of S-methyldithiocarbazate (H₂L²), the 2-hydroxy-5-nitrobenzaldehyde Schiff base of S-methyldithiocarbazate (H₂L³), and the 2-hydroxy-5-nitrobenzaldehyde Schiff base of S-benzyldithiocarbazate (H₂L⁴), and their complexes of general formula [Ni(HL¹)₂], [ML] (M?=?Ni^II or Cu^II; L?=?L¹, L², L³ and L⁴), [Co(HL)(L); L?=?L¹, L², L³ and L⁴] and [ML(B)] (M?=?Ni^II or Cu^II; L?=?L² and L⁴; B?=?py, PPh₃) have been prepared and characterized by physico-chemical techniques. Spectroscopic evidence indicates that the Schiff bases behave as ONS tridentate chelating agents. X-ray crystallographic structure determination of [NiL²(PPh₃)] and [CuL⁴(py)] indicates that these complexes have an approximately square-planar structure with the Schiff bases acting as dinegatively charged ONS tridentate ligands coordinating via the phenoxide oxygen, azomethine nitrogen and thiolate sulfur atoms. The electrochemical properties of the complexes have been studied by cyclic voltammetry.     

ZnO nanoparticles and poly(acrylic) acid-based polymer gel electrolyte for photo electrochemical cell

This work presents a photo electrochemical cell based on zinc oxide (ZnO) nanoparticles and poly(acrylic) acid (PAA) doped with sodium iodide (NaI) and iodine (I₂) polymer gel electrolyte. The ZnO powders were synthesized by sol–gel storage and sol–gel centrifugation. The ZnO powder synthesized via sol–gel centrifugation showed the optimal structural properties, with largest crystallite sizes of 58 nm, average particles size between 20 and 80 nm and indirect band gap energy of 3.20 eV. The highest conductivity [(8.0 ± 0.1) × 10^?2 S cm^?1] was obtained for PAA + 0.8 M NaI + 0.02 M I₂. This sample achieved the lowest activation energy (0.029 eV) and electrochemical stability at 1.6 V. The ZnO powder synthesized via sol–gel centrifugation and PAA + 0.8 M NaI + 0.02 M I₂ was fabricated as a Cu–ZnO/PAA + 0.8 M NaI + 0.02 M I₂/C-ITO photo electrochemical cell.     

A new piezoelectric response model for population growth of bacteria

A piezoelectric response model on the population growth of microorganism is proposed. This model is based on a novel population growth model, which has a more obvious ecological meaning and the fact that the series piezoelectric quartz crystal (SPQC) sensor responses to conductivity changes of the medium during the growth of the microorganism. From the response model four parameters can be obtained including the maximum specific growth rate mu(m), saturated population size N(m), and two constants C and K(1). The influence of the parameters on the response curve is discussed in which the influences of mu(m) and N(m) are more obvious. With the proposed model the quantitative determination of bacteria may be more accurate than the frequency detection time (FDT) method. Then the growth of Escherichia coliform (E. coli) monitored with a SPQC sensor is compared with the simulated growth curve obtained by the proposed model and a good agreement is obtained.     

Facile Fabrication of a Graphene‐based Electrochemical Biosensor for Glucose Detection

A simple and effective glucose biosensor based on immobilization of glucose oxidase (GOD) in graphene (GR)/Nafion film was constructed. The results indicated that the immobilized GOD can maintain its native structure and bioactivity, and the GR/Nafion film provides a favorable microenvironment for GOD immobilization and promotes the direct electron transfer between the electrode substrate and the redox center of GOD. The electrode reaction of the immobilized GOD shows a reversible and surface‐controlled process with the large electron transfer rate constant (k_s) of 3.42±0.08 s^?1. Based on the oxygen consumption during the oxidation process of glucose catalyzed by the immobilized GOD, the as‐prepared GOD/GR/Nafion/GCE electrode exhibits a linear range from 0.5 to 14 mmol·L^?1 with a detection limit of 0.03 mmol·L^?1. Moreover, it displays a good reproducibility and long‐term stability.     

Alcohol‐Processable Organic Amorphous Electrolytes as an Effective Electron‐Injection Layer for Organic Light‐Emitting Diodes

A new series of monoammonium‐based organic electrolytes with the tetrafluoroborate (BF₄^?) counteranion have been synthesized. Replacing the pendant ethyl groups in the fluorenyl unit with 4‐ethoxyphenyl groups dramatically improves both solubility and morphological stability. The characterization of the alcohol‐processable amorphous ionic compounds as an electron‐injection layer in organic light‐emitting diodes (OLEDs) reveals that the organic electrolyte that comprises a rigid linear‐conjugated unit provides better device performance, with respect to its counterpart containing a branched bulky moiety. The capability of these compounds to facilitate electron injection from air‐stable aluminum metal is preliminarily discussed on the basis of the investigations of the electron‐only devices and photovoltaic experiments.