In situ derivatization and hollow‐fiber liquid‐phase microextraction to determine sulfonamides in water using UHPLC with fluorescence detection

A sensitive method for determining sulfonamides in water was developed and validated through in situ derivatization and hollow‐fiber liquid‐phase microextraction with ultra‐high performance liquid chromatography and fluorescence detection. The target sulfonamides were sulfadiazine, sulfacetamide, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfamethoxazole, and sulfisoxazole. Following in situ derivatization with fluorescamine, three‐phase hollow‐fiber liquid‐phase microextraction with an S 6/2 polypropylene hollow‐fiber membrane was applied automatically using a multipurpose autosampler. Experimental parameters including derivatization time, choice of organic phase, pH of donor and acceptor phase, stirring rate, extraction temperature and time were optimized. Under optimized conditions, the target sulfonamides achieved excellent linearity with correlation coefficients of 0.9924–0.9994 within the concentration range of 0.05–5 μg/L. The limits of detection of the eight sulfonamides were 3.1–11.2 ng/L, and the limits of quantification were 10.3–37.3 ng/L. Enrichment factors of 0.1 and 5 μg/L sulfonamides spiked in lake water were 14–60, and recoveries were 56–113% with relative standard derivations of 3–19%. Applied with the developed method, sulfamerazine and sulfamethoxazole were measurable in both influent and effluent water of the three sewage treatment plants in Guangzhou, China. The developed method was sensitive and provided an alternative method for simultaneously enriching and quantifying multiple sulfonamides in environmental water.     

Adsorbed hollow fiber‐based biological fingerprinting for the discovery of platelet aggregation inhibitors from Danshen–Honghua decoction

For lead compound discovery from natural products, hollow fiber cell fishing with chromatographic analysis is a newly developed method. In this study, an adsorbed hollow fiber‐based biological fingerprinting method was firstly developed to discover potential platelet aggregation inhibitors from Danshen–Honghua decoction. Platelets were seeded on the fiber and their survival rate was tested. Results indicated that more than 92% platelets survived during the whole operation process. Ranitidine and tirofiban were used as positive and negative control respectively to verify the reliability of the presented approach. The main variables such as amount of extract and stirring time that affect the adsorbed hollow fiber‐based biological fingerprinting process were optimized, and the repeatability of this method was also investigated. Finally, 12 potential active compounds in Danshen–Honghua decoction were successfully detected using the established approach and structures for nine of them were tentatively identified by liquid chromatography with mass spectrometry analysis. In addition, the in vitro platelet aggregation inhibition test was carried out for five of the nine hit compounds, and three active components, namely, lithospermic acid, salvianolic acid A, and salvianolic acid B were confirmed. These results proved that the proposed method could be an effective approach for screening platelet inhibitors from plant extracts.     

Protonation of polyaniline‐coated silica stationary phase affects the retention behavior of neutral hydrophobic solutes in reversed‐phase capillary liquid chromatography

Because of its high conductivity when acid doped, polyaniline is known as a synthetic metal and is used in a wide range of applications, such as supercapacitors, biosensors, electrochromic devices, or solar and fuel cells. Emeraldine is the partly oxidized, stable form of polyaniline, consisting of alternating diaminobenzenoid and iminoquinoid segments. When acidified, the nitrogen atoms of emeraldine become protonated. Due to electrostatic repulsion between positive charges, the polarity and morphology of emeraldine chains presumably change; however, the protonation effects on emeraldine have not yet been clarified. Thus, we investigated these changes by reversed‐phase capillary liquid chromatography using a linear solvation energy relationship approach to assess differences in dominant retention interactions under a significantly varied mobile phase pH. We observed that hydrophobicity dominates the intermolecular interactions under both acidic and alkaline eluent conditions, albeit to different extents. Therefore, by tuning the mobile phase pH, we can even modulate the retention of neutral hydrophobic solutes, such as aromatic hydrocarbons, because the pH‐dependent charge and structure of polymer chains of the emeraldine‐coated silica stationary phase show a mixed‐mode separation mechanism.     

Preparation and characterization of glass fiber–reinforced polyethylene terephthalate/linear low density polyethylene (GF‐PET/LLDPE) composites

Polyethylene terephthalate (PET) was melt blended with linear low density polyethylene (LLDPE) and subsequently compounded with glass fibers (GF) as reinforcements at percentages ranging from 15 to 45 wt% of LLDPE and 5 to 30 wt% of GF. Thermal, morphological, and mechanical properties of the prepared composites were investigated. It was found that compounding PET/LLDPE blends with GF would be beneficial in producing composites that are thermally stable with good mechanical properties. For example, the impact strength of the composites containing 85/15 wt% (PET/LLDPE) at relatively high loading of GF, ie, from 15 to 30 wt%, was higher than that of the GF‐reinforced neat PET. When increasing the percentage of LLDPE in the composites, the impact strength increased with increasing GF content, and this was also better than that of GF‐reinforced PET whose impact strength drastically decreased upon increasing the GF%. The improvement in mechanical properties of the composite, we suggest, should be correlated with the morphologies of the composites where the visualized interface adhesion tended to be better at higher loadings of both LLDPE and GF.     

纳米锰基普鲁士白的制备及电化学储钠性能

采用高温共沉淀法制备锰基菱方相的普鲁士白正极材料,研究合成温度对产物微结构和电化学性能的影响。研究发现,随着合成温度的提高,产物的结晶度、颗粒尺寸和嵌钠容量明显提高。当合成温度为90℃时,产物在15 mA·g^-1下首次充放电容量分别达到142和139 mAh·g^-1。在30和50 mA·g^-1分别循环300和600次时,容量仍保持在111和89 mAh·g^-1。     

Determination of Trace Elements in Dendrobium Officinale Cultivated in Various Conditions

Dendrobium officinale is an important medicinal plant in traditional Chinese medicine. The consumption of D. officinale has increased rapidly in recent years due to the health awareness among Chinese people. The present study aimed to determine trace elements levels in 42 D. officinale samples and to utilize the elemental data for identifying the cultivation technique. Eighteen trace elements (B, V, Cr, As, Mn, Fe, Mo, Cu, Zn, Se, Sr, Sn, Ti, Al, Co, As Pb, Cd, and Bi) were determined by inductively coupled plasma–mass spectrometry. Of the 11 essential elements, the mean concentrations ranged from 30.6?µg?kg^?1 (Mo) in D. officinale with greenhouse cultivation to 161?mg?kg^?1 (Fe) in D. officinale with rock cultivation, and the contributions of Mn may exceed the dietary reference intake value by the uptake of 20?g of D. officinale. Of the seven toxic elements, the mean concentrations ranged from 3.29?µg?kg^?1 (Bi) in the D. officinale with greenhouse cultivation to 342?mg?kg^?1 (Al) in the D. officinale with rock cultivation, and the contributions of Al may exceed the provisional tolerable daily intake value by the uptake of 20?g of D. officinale. The concentrations of seven metals (Bi, Pb, Fe, Al, Cr, As, and Mo) were utilized to identify the cultivation technique of the analyzed D. officinale samples through linear discriminant analysis.     

三元镍钴锰正极材料的制备及改性

三元镍钴锰正极材料是一类非常重要的正极材料,具有性能优于钴酸锂而成本远远低于钴酸锂、能量密度远远高于磷酸铁锂等重要优点,正在逐渐成为汽车动力电池的主流正极材料。但是,三元镍钴锰正极材料也存在循环稳定性不足、大电流密度放电性能不佳等问题。围绕解决这些问题并进一步提升三元镍钴锰正极材料的性能,近年来国内外在材料制备技术以及改性技术方面开展了大量的研究工作,取得了若干令人瞩目的研究成果。本文从材料制备方法、包覆修饰和掺杂改性三个方面,介绍了三元镍钴锰正极材料制备技术及改性技术的研究进展,在此基础上,对三元镍钴锰正极材料的未来发展方向作出展望。     

超高效液相色谱-线性离子阱/静电场轨道阱质谱法快速检测化妆品中66种抗生素

采用超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱法同时测定化妆品中磺胺类、沙星类等66种抗生素类化合物,建立了快速筛查数据库和定量分析方法。待测物用乙腈超声提取,C18色谱柱（100 mm×2.1 mm,1.8 μm）分离,以0.1%（v/v）甲酸水溶液和乙腈为流动相进行梯度洗脱。在正离子模式下,以保留时间和一级母离子精确质量数进行快速筛查,以高能碰撞诱导解离获得的二级碎片离子精确质量数进行确证。结果表明,化合物的线性关系良好,线性相关系数（R²）>0.99;检出限（LOD）为2~4 μg/kg;定量限（LOQ）为5~10 μg/kg;3个添加水平（1LOQ、10LOQ、30LOQ）的平均回收率为58.2%~119.1%,相对标准偏差为1.03~11.9%。该方法简便快速、定性定量可靠,适用于化妆品中抗生素类化合物的快速筛查和定量检测。