黑米花色苷酰化修饰红外光谱分析

黑米花色苷易受外部环境影响发生降解致使局部分子结构破坏而使营养价值和保健功能有所下降。利用有机酸提供酰基对黑米花色苷进行修饰来提高花色苷结构的稳定性。利用红外光谱分析经咖啡酸酰化修饰黑米花色苷的结构变化。结果表明：黑米花色苷酰化修饰前后于官能团区3 650~3 200和1 680~1 620 cm-1处均有吸收峰，且其于指纹区1 282.68和1 277.51 cm-1处出现酚羟基吸收峰，于1 056.07和1 054.03 cm-1处出现醇羟基吸收峰，719.90和719.71 cm-1处出现苯环上C-H面外弯曲振动吸收峰。由此可见，黑米花色苷酰化修饰后主要结构框架仍为花色苷的芳环结构。此外，黑米花色苷酰化修饰前后于1 900~1 650 cm-1间1 714.28和1 728.13 cm-1处均出现共轭羰基的特征吸收峰，对应于可直接连接在苯环上的α-羰基结构，由此说明黑米花色苷结构中存在着酰基基团。黑米花色苷经酰化修饰后红外图谱于1 517.20 cm-1处出现新吸收峰，其正好处于1 800~900 cm-1双键(不含氢)伸缩振动区，指纹区876.65 cm-1处亦出现了苯环上的C-H面外弯曲振动吸收峰。与之相呼应在经二阶导数处理后红外光谱图中在2 500～2 000 cm-1间出现了新的波动，此波段为累积双键伸缩振动区，而官能团区3 650~3 200 cm-1间3 370.20 cm-1处的吸收峰正好处于多分子缔合区。由此可见，在咖啡酸作为酰基供体，酰化修饰黑米花色苷时由于分子间的重新缔合于结构中引入了新的酰基基团而呈现出一种双酰化的空间结构。黑米花色苷酰化结构中有机酸与糖链相连，将有机酸置于2-苯基苯并吡喃骨架的表面，这种堆积作用模式可以较好地抵抗水的亲核攻击和其他降解反应进而提高黑米花色苷结构的稳定性。     

浅谈黄原胶及其在农药制剂加工中的应用

黄原胶是极具发展潜力的生物多糖,独特的分子结构使其具有良好的增稠、乳化和稳定作用,已被广泛应用于日用化工、石油开采、纺织印染、食品、医药、涂料、农药等众多工业领域,拥有广阔的市场前景。本文对黄原胶的结构、特性、生产工艺以及主要应用领域等进行了简单综述,总结了黄原胶在农药制剂加工中的应用现状,指出黄原胶优越的流变特性对悬浮剂、水乳剂、悬乳剂等农药制剂悬浮稳定性的提高具有重大意义,最后展望了黄原胶未来的发展前景。     

A study of fluorescence properties of citrinin in β-cyclodextrin aqueous solution and different solvents

Citrinin (CIT) is a nephrotoxic mycotoxin initially isolated from filamentous fungus Penicilliu citrinum. It was later isolated from several other species, such as Aspergillus and Monascus. It has a conjugated, planar structure that gives it a natural fluorescence ability, which can be used to develop sensitive methods for detecting CIT in food. In this paper, we used the spectro?uorescence technique to study the effects of pH value, β-cyclodextrin (β-CD) and organic solvents on the CIT fluorescence intensity. The results show that lower pH value, aceitc acid, β-CD and acetonitrile can induce a higher fluorescence intensity of CIT, but methanol or H₂O has a decreasing effect on the fluorescence intensity of CIT. Findings in this study provide a theoretical basis for development of a high sensitivity fluorescence-based trace analysis for CIT detection.     

Optical properties of ZnS–carbon nanotubes composites

In this work we present a study of growth and characterization of ZnS/carbon nanotube (CNT) composites. The composites were prepared with a chemical mix technique and characterized by SEM analysis, Auger Electron Spectroscopy (AES) and Cathodoluminescence (CL) spectroscopy. The analyses show that the sample is formed by a direct contact between CNT and zinc sulfide. In particular, SEM images show CNTs wrapped around ZnS micrometer particles. Furthermore, AES spectroscopy shows the absence of chemical bonds between ZnS and CNT and that the sample homogeneity increases with the CNT amount in the composite.Finally CL studies show that our composites present a visible luminescence signal centered at about 500 nm, with a shift of luminescence emission peak linked to the amount of CNT in the sample.     

不同夹带剂对3种丹参酮超临界CO2流体萃取效果的影响

使用不同夹带剂,用超临界CO₂流体萃取丹参中3种丹参酮,研究不同夹带剂的萃取效果。在优化操作条件下萃取丹参中3种丹参酮,HPLC测定萃取物中3种丹参酮的质量分数。3种夹带剂中,95%（V/V）极性物质乙醇效果最好,其次为丙酮、正辛烷。用超临界CO₂流体萃取丹参中3种丹参酮,为了提高萃取率,须使用极性溶剂乙醇作为夹带剂。     

Determination of hydroxysafflor yellow A in biological fluids of patients with traumatic brain injury by UPLC‐ESI‐MS/MS after injection of Xuebijing

A simple, novel, specific, rapid and reproducible ultra‐performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for the determination of hydroxysafflor yellow A (HSYA) in biological fluids (plasma, urine and cerebrospinal fluid) of patients with traumatic brain injury after intravenous injection of Xuebijing (XBJ). Liquid–liquid extraction was performed, and separation was carried out on an Acquity UPLC? BEH C₁₈ column, with gradient elution using a mobile phase composed of methanol and 0.1% formic acid at a flow rate of 0.3 mL/min. A triple quadrupole tandem mass spectrometer with electrospray ionization was used for the detection of HSYA. The mass transition followed was m/z 611.0 → 491. The retention time was less than 3.0 min. The calibration curve was linear in the concentration range from 2 to 6125 ng/mL for cerebrospinal fluid, plasma and urine. The intra‐ and inter‐day precisions were <10%, and the relative standard deviation of recovery was <15% for HSYA in biological matrices. The method was successfully applied for the first time to quantify HSYA in the biological fluids (especially in cerebrospinal fluid) of patients with traumatic brain injury following intravenous administration of XBJ. Copyright © 2014 John Wiley & Sons, Ltd.     

Dissipation,residue, and distribution of pyraclostrobin in banana and soil under field conditions in South China

Two independent field trials were conducted in Guangdong and Guangxi, South China, in 2013, to study the dissipation, residue levels, and distribution of pyraclostrobin in banana and soil under field conditions. Pyraclostrobin residues were determined through a quick and effective method of high-performance liquid chromatography. Results showed that the average recoveries ranged from 80.55% to 98.08%, with relative standard deviations of 3.18–7.81% at three different spiking levels for each different matrix. The quantification limit of the proposed method was 0.006 mg/kg for both banana and soil. The half-lives of pyraclostrobin in bananas were 9.09 days in Guangdong and 8.26 days in Guangxi, and both bananas exhibited a dissipation rate of 90% after 28 days. The half-lives of pyraclostrobin in soil were 11.61 days in Guangdong and 10.60 days in Guangxi, with a dissipation rate of 90% after 35 days. Although several positive banana samples (i.e., pyraclostrobin exceeding the maximum residue limits (MRL) were found, the terminal residues in banana pulp were not detectable. All the terminal residues in banana pulp were below the MRL of 0.02 mg/kg, set by the Chinese Ministry of Agriculture, indicating a negligible risk associated with the exposure to pyraclostrobin via the consumption of banana. The distribution of pyraclostrobin in soil was also investigated in two experimental sites. The pyraclostrobin in different layer soil was time dependent and did not vary between the two sites. The result also showed that pyraclostrobin could be easily transported from the top soil to the subsoil. However, the highest quantity ratio did not exceed 10% in the bottom layer (20–30 cm). The distribution assessment also revealed that no significant potential environment risk was induced by pyraclostrobin in bananas.     

Film-forming characteristics and thermal stability of low viscosity benzoxazines derived from melamine

A novel class of low-viscosity benzoxazines has been synthesized from melamine and formaldehyde with phenol or bisphenol A. The striking feature of the class of benzoxazines is the subtle combination of their inherently low viscosity at room temperature, good film-forming characteristics and high chemical and thermal stability mainly due to the introduction of melamine into the network of the polymers. The structure of the benzoxazines has been confirmed by proton nuclear magnetic resonance spectroscopy and fourier transform infrared spectroscopy. Thermal properties of polybenzoxazine have been studied by differential scanning calorimetry, dynamic mechanical analysis and thermogravimetric analysis. Transparent polybenzoxazine films were easily obtained under solvent-free conditions, exhibiting significantly improved toughness compared to the conventional polybenzoxazines. Our research may open a new path for overcoming the present drawbacks of polybenzoxazines such as high brittleness, the difficulties in preparing films and poor processibility via tailoring the structures and properties of amine in the benzoxazines.     

Synthesis of tetrazole containing 1,2,3-thiadiazole derivatives via U-4CR and their anti-TMV activity

A series of novel tetrazole containing 1,2,3-thiadiazole derivatives were designed and synthesized via Ugi reaction. Their structures were confirmed by melting points, IR, 1H NMR, and HRMS (ESI). Preliminary bioassay indicated that most target compounds exhibited very good direct anti-TMV activity at 100 μg/mL, which was equal to or higher than that of ribavirin. Among them, compounds 4b, 4c and 4i also showed equivalent protection effect to ribavirin in vivo at 100 μg/mL.     

Dissipation of the plant growth regulator hexanoic acid 2-(diethylamino) ethyl ester in pakchoi and soil

A rapid and simple method for determining the plant growth regulator hexanoic acid 2-(diethylamino) ethyl ester (DA-6) in pakchoi and soil using gas chromatography-mass spectrometry (GC-MS) has been developed. For this purpose, a single step was used to extract DA-6 with dichloromethane from aqueous-acetone extracts of vegetables and soil. Average recoveries of DA-6 in pakchoi and soil were between 85% and 104% at both spiking levels 0.01 and 0.1 mg kg^?1. Relative standard deviations (RSD) were less than 11% for all of the recovery tests. The degradation of DA-6 in pakchoi and soil was studied. The results showed that DA-6 degradation in pakchoi and soil coincided with C = 3.9903 e^{?0.0516 t} , C = 0.3476 e^{?0.0224 t} , respectively; the half-lives were 13.43 h and 30.94 h in pakchoi and soil in Beijing, respectively.