通过RRLC-Q-TOF MS和UPLC-QQQ MS分析原人参三醇型皂苷在人肠道菌群中的代谢产物

通过高分离度快速液相色谱-四极杆飞行时间质谱(RRLC-Q-TOF MS)和超高效液相色谱-三重四极杆质谱(UPLC-QQQ MS)法对原人参三醇型皂苷Re、Rg 1、Rg 2、Rh 1、Rf、F 1、R 1在人肠道菌群中的转化产物进行定性、定量分析,确定原人参三醇型皂苷的代谢产物、转化途径和60 h时的转化率。结果表明,人参皂苷Re的转化产物为人参皂苷Rg 1、Rg 2、Rh 1、F 1和PPT,转化率为91%;人参皂苷Rg 1的转化产物为人参皂苷Rh 1、F 1和PPT,转化率为80%;人参皂苷Rg 2的转化产物为人参皂苷Rh 1和PPT,转化率为73%;人参皂苷Rh 1和F 1主要通过PPT代谢,转化率分别为82%和81%;人参皂苷Rf的转化产物为人参皂苷Rh 1和PPT,转化率为89%;三七皂苷R 1的转化产物为人参皂苷Rg 1、R 2、Rh 1和PPT,转化率为79%。原人参三醇型皂苷类成分可被人肠道菌群代谢,主要通过丢失糖残基形成转化产物,而次级皂苷和苷元是人参在体内发挥药理作用的物质基础。     

Controllable layer-by-layer assembly based on brucite and alginates with the assistance of spray drying and flame retardancy influenced by gradients of alginates

With the aim of tailoring and controlling surface assembly, multifunctional flame retardants (FRs) were obtained based on depositing alginates and silane coupling agents on brucite via the spray-drying-assisted layer-by-layer assembly technique. The assembly was controllable in both structure and gradient mass. Two series of FRs were named CuFR1-3 and NiFR1-3 based on the assembly content of metal alginates. With the assistance of spray drying, good compatibility between FRs and ethylene-vinyl acetate (EVA) was obtained, resulting in better mechanical properties. Meanwhile, the FRs improved flame retardancy and smoke suppression when used in EVA composites. With 55 wt % loading, composites with CuFR3 and NiFR1 passed UL 94 V-0 rating, while those with brucite were not rated. The peak of heat release rate decreased by 51.7 and 49.3% while the residue increased by 9.8 and 11.9%, respectively. The FRs also reduced the smoke and CO production rates. For the two series of FRs, the relationship between FR efficiency and alginate contents is different. The CuFRs assembled more copper alginates and exerted better flame retardancy caused by lower catalytic graphitization. NiFRs exerted a higher catalyzing efficiency at low assembly content. However, at high assembly content, the catalytic graphitization effect would decrease by thermally oxidized degradation leading to excess nickel alginates. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 47570.     

氢化物原子荧光光谱法测定酱油中微量铅的方法研究

建立了一种快速、高效的QuEChERS-高效液相色谱-质谱联用法（QuEChERS-HPLC-MS/MS）测定谷类杂粮制品中脱氧雪腐镰刀菌烯醇（DON）、3-乙酰脱氧雪腐镰刀菌烯醇（3-ADON）、15-乙酰脱氧雪腐镰刀菌烯醇（15-ADON）和玉米赤霉烯酮（ZON）共4种真菌毒素。样品前处理采用乙腈-水溶剂提取，经Florisil+C18+无水硫酸镁净化后检测。以0.10%甲酸-乙腈作为流动相，在质谱检测器的多反应监测模式下进行分析。结果表明，4种真菌毒素在各自的线性范围内线性关系良好，相关系数R2均大于0.999，回收率在85.1%～102.0%，相对标准偏差（RSD）为2.11%～6.22%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于谷类杂粮制品中DON、3-ADON、15-ADON 和ZON的分析和定量检测。     

便携式飞行时间质谱仪的研制及其在石化污水系统挥发性有机物监测中的应用

近年来，国内的大气污染问题越来越严重，挥发性有机物（VOCs）的排放是其中一个重要原因。VOCs是臭氧和气溶胶的前驱物之一，在大气化学反应过程中扮演着极其重要的角色。本实验自行研制了一台基于真空紫外（VUV）灯的高分辨光电离飞行时间质谱仪（TOF MS），建立了一种新的VOCs稀释采样方法，并将其应用于石化行业污水处理系统VOCs的采样与分析。结果表明：隔油系统的3个池子基本没有测到高浓度的挥发性有机物，其中溶气气浮甲苯物质的质量浓度最高，为50.41 mg/L，其余组分的质量浓度大多数在0.1~1.0 mg/L之间；1#加氢和2#加氢隔油池有着类似的组分浓度，以1#加氢隔油池为例，二甲苯物质的质量浓度为10.60 mg/L，乙苯为52.33 mg/L，苯为59.80 mg/L；由于罐区隔油池没有加盖，处于露天状态，挥发性有机物气体容易向大气中扩散，并没有检测出较高浓度组分。可以看出，新式采样方法可有效地稀释定量样品，操作简便，减少了样品因闪蒸过程造成的VOCs损失，检出物质更丰富；同时，使用自行研制的TOF MS仪器能够快速检测不同装置污水处理系统的VOCs种类，将该仪器用于实际样品检测，发现化工企业大多数密闭的池子都含有苯系物、醚类等，但不同工艺的污水处理系统VOCs存在明显差异。该质谱仪适用于石化企业污水系统VOCs监测。     

Enhanced high-temperature dielectric properties and microwave absorption of SiC nanofibers modified Si3N4 ceramics within the gigahertz range

Si₃N₄ ceramics modified with SiC nanofibers were prepared by gel casting aiming to enhance the dielectric and microwave absorption properties at temperatures ranging from 25?°C to 800?°C within X-band (8.2–12.4?GHz). The results indicate that the complex permittivity and dielectric loss are significantly increased with increased weight fraction of SiC nanofibers in the Si₃N₄ ceramics. Meanwhile, both complex permittivity and dielectric loss of SiC nanofibers modified Si₃N₄ ceramics are obviously temperature-dependent, and increase with the higher test temperatures. Increased charges mobility along conducting paths made of self-interconnected SiC nanofibers together with multi-scale net-shaped structure composed of SiC nanofibers, Si₃N₄ grains and micro-pores are the main reason for these enhancements in dielectric properties. Moreover, the calculated microwave absorption demonstrates that much enhanced microwave attenuation abilities can be achieved in the SiC nanofibers modified Si₃N₄ ceramics, and temperature has positive effects on the microwave absorption performance. The SiC nanofibers modified Si₃N₄ ceramics will be promising candidates as microwave absorbing materials for high-temperature applications.     

The influence of carbon materials on the absorption performance of polymer-derived SiCN ceramics in X-band

Carbon-containing polymer-derived SiCN ceramics (PDCs-SiCN-C) were successfully fabricated with multi-layer graphene (MLG) and multiwalled carbon nanotubes (MWCNTs) as additives at 1100?°C. The effects of MLG and MWCNTs on the microwave absorption properties of PDCs-SiCN-C ceramics were analyzed. The imaginary permittivity and loss tangent of SiCN-MLG and SiCN-MWCNTs were about 3.4, 0.67 at 11.2?GHz and 3.1, 0.57 at 10.6?GHz, respectively. The minimum reflection loss of SiCN-MLG and SiCN-MWCNTs at 3?mm was ??54?dB and ??48?dB with the effective absorption bandwidth (RL ≤ ?10?dB, >90% absorption) about 1.5?GHz and 0.9?GHz in X-band.     

Surface sedimentation and adherence of Nano‐SiO2 to improve thermal stability and flame resistance of melamine‐formaldehyde foam via sol‐gel method

Melamine‐formaldehyde foam possesses intrinsic flame retardance; however, relative poor thermal stability and a certain amount of heat release rate restrict its applications in heated environment to a degree. In the present research, sol‐gel method has been adopted to precipitate nano‐SiO₂ particles on the surface of the melamine‐formaldehyde foam's fibers to construct a protective inorganic gel layer. Taking advantages of the shielding effects of the gel layer, the thermal‐oxygen degradation of the foam can be greatly retarded during heating; hence, the thermal stability is remarkably improved, and the flame retardance is further enhanced. In addition, introducing a small amount of membrane‐forming agent in the sol‐gel system can make the depositional nano‐SiO₂ particles well adhered to avoid dusting.     

Mullite-bonded SiC-whisker-reinforced SiC matrix composites: Preparation,characterization, and toughening mechanisms

A novel mullite-bonded SiC-whisker-reinforced SiC matrix composite (SiCw/SiC, SiC whisker-to-SiC powder mass ratio of 1:9) was designed and successfully prepared. Before preparing the composite, the inexpensive lab-made SiCw was first modified by an oxidation/leaching process and then coated with Al₂O₃. The kinetics results indicate that the oxidation process can be described by improved shrinking-cylinder models. The aspect ratio of SiCw improved after modification. Subsequently, raw materials with a SiC–SiO₂–Al₂O₃ triple-layered structure were obtained after the Al₂O₃-coating process and used as feedstocks during the subsequent hot-pressing sintering. Finally, the characterization of the composites indicates that the mullite-bonded sample performs better (relative density of 93.8?±?1.4%, flexural strength of 533.3?±?18.2?MPa, fracture toughness of 13.6?±?2.1?MPa?m^1/2, and Vickers hardness of 20.6?±?2.5?GPa) than the reference sample without the mullite interface. The improved toughness could essentially be attributed to the moderately strong interface bonding and effective load transfer effects of the mullite interface.     

Synergistic flame retardant effects of activated carbon and molybdenum oxide in poly(vinyl chloride)

The synergistic effects of activated carbon (AC) and molybdenum oxide (MoO₃) in improving the flame retardancy of poly(vinyl chloride) (PVC) were investigated. The effects of AC, MoO₃ and their mixture with a mass ratio of 1:1 on the flame retardancy and smoke suppression properties of PVC were studied using the limiting oxygen index and cone calorimeter tests. It was found that the flame retardancy of the relatively cheaper AC was slightly weaker than that of MoO₃. In addition, the incorporation of AC and MoO₃ greatly reduced the total heat release and improved smoke suppressant property of PVC composites. When the total content of AC and MoO₃ was 10 phr, PVC/AC/MoO₃ had the lowest peak heat release rate and peak smoke production rate values of 173.80 kW m^?2 and 0.1472 m² s^?1, which represented reductions of 47.3 and 59.9%, respectively, compared with those of PVC. Furthermore, thermogravimetric analysis and gel content tests were used to analyze the flame retardant mechanism of AC and MoO₃, with results showing that AC could promote early crosslinking in PVC. Char residue left after heating at 500 °C was analyzed using scanning electron microscopy and Raman spectroscopy, and the results showed that MoO₃ produced the most compact char, with the smallest and most organized carbonaceous microstructures. © 2017 Society of Chemical Industry