高效液相色谱法测定化妆品中依克多因的含量

建立高效液相色谱法测定化妆品中依克多因的分析方法,采用Agilent Poroshell 120 EC-C₁₈色谱柱（100 mm×3.0 mm,2.7μm）分离,以甲醇和p H为3.0的40 mmol/L磷酸二氢钠-10 mmol/L 1-庚烷磺酸钠缓冲溶液梯度洗脱,流速0.8 m L/min,柱温30℃,检测波长210 nm。采用外标法定量测定化妆品中的依克多因含量。结果表明,依克多因在5～800 mg/L的质量浓度范围内呈现良好线性关系,相关系数为0.999 8,方法的检出限和定量限分别为0.3和1.0 mg/L。该方法具有分离效率高、分析时间短、节省溶剂等优点,解决了依克多因在C₁₈色谱柱上保留弱的问题。     

Cheese ripening in nonconventional conditions: A multiparameter study applied to Protected Geographical Indication Canestrato di Moliterno cheese

A multiparameter study was performed to evaluate the effect of fondaco, a traditional ripening cellar without any artificial temperature and relative humidity control, on the chemical, microbiological, and sensory characteristics of Protected Geographical Indication Canestrato di Moliterno cheese. Ripening in such a nonconventional environment was associated with lower counts of lactococci, lactobacilli, and total viable bacteria, and higher presence of enterococci, in comparison with ripening in a controlled maturation room. Moreover, fondaco cheese underwent accelerated maturation, as demonstrated by faster casein degradation, greater accumulation of free AA, and higher formation of volatile organic compounds. Secondary proteolysis, as assessed by liquid chromatography-mass spectrometry of free AA and low molecular weight peptides, did not show any qualitative difference among cheeses, but fondaco samples evidenced an advanced level of peptidolysis. On the other hand, significant qualitative differences were observed in the free fatty acid profiles and in the sensory characteristics. Principal component analysis showed a clear separation of the fondaco and control cheeses, indicating that ripening in the natural room conferred unique sensory features to the product.     

超高效液相色谱⁃四极杆⁃飞行时间质谱对含PET食品接触材料中可迁移非挥发性物质的筛查研究

采用超高效液相色谱⁃四极杆⁃飞行时间高分辨质谱（UPLC⁃Q⁃TOF）对4类不同类型的含聚对苯二甲酸乙二醇酯（PET）材质的食品接触材料在4 %乙酸和50 %乙醇模拟物中的迁移出的非挥发性未知物进行筛查解析。结果表明，产品在4 %乙酸模拟物的迁移风险远小于50 %乙醇模拟物，主要迁移物质为聚合单体形成的寡聚物，抗氧剂、润滑剂、胶黏剂等加工助剂以及生产加工、迁移过程中形成的非有意添加物（NIAS）物质；纯PET材质的产品迁移物质较少，多层复合材料迁移物质较多。复合材质的产品中，PET材质可能在生产时添加了己二酸、癸二酸、新戊二醇等物质，进行了改性处理；此外，部分迁移物质会与模拟物中的乙醇发生反应，生成新的NIAS物质。     

Synthesis of Ti3C2Fx MXene with controllable fluorination by electrochemical etching for lithium-ion batteries applications

Ti₃C₂T_x MXene has attracted remarkable attention due to its promising applications in energy storage and sensors. However, traditional MXene preparation methods used HF as etchant, which was highly toxic and harmful to human and environment. Moreover, the aqueous etchants will also result in the combination of OH, O and F groups on the surfaces, making it difficult to control the varieties and contents of the surface terminations. In this paper, a green and mild electrochemical exfoliation method was proposed to synthesize Ti₃C₂F_x and synchronously control its fluorination degree on the surface. A non-aqueous ionic liquid, [BMIM][PF₆]-based solution was used as electrolyte. The as-prepared Ti₃C₂F_x was fluorinated with the CF and TiF₃ groups, which were electrochemically active and contributed to the excellent cycling stability of the MXene anode-based Li-ion batteries. These findings provided a facile strategy to prepare MXene materials and dope MXene with tailored property for MXene-based energy devices applications.     

Microstructural and mechanical properties assessment of transient liquid phase bonding of CoCuFeMnNi high entropy alloy

The transient liquid phase (TLP) bonding of CoCuFeMnNi high entropy alloy (HEA) was studied. The TLP bonding was performed using AWS BNi-2 interlayer at 1050 °C with the TLP bonding time of 20, 60, 180 and 240 min. The effect of bonding time on the joint microstructure was characterized by SEM and EDS. Microstructural results confirmed that complete isothermal solidification occurred approximately at 240 min of bonding time. For samples bonded at 20, 60 and 180 min, athermal solidification zone was formed in the bonding area which included Cr-rich boride and Mn₃Si intermetallic compound. For all samples, the γ solid solution was formed in the isothermal solidification zone of the bonding zone. To evaluate the effect of TLP bonding time on mechanical properties of joints, the shear strength and micro-hardness of joints were measured. The results indicated a decrement of micro-hardness in the bonding zone and an increment of micro-hardness in the adjacent zone of joints. The minimum and maximum values of shear strength were 100 and 180 MPa for joints with the bonding time of 20 and 240 min, respectively.     

堆本体抗震试验动力相似关系推导与验证

为确保堆本体抗震试验中流体对流效应、脉冲效应和堆本体结构响应的准确性，需保证重力、流体与固体惯性力、结构弹性力和结构应变的相似性。本文从固体结构的振动方程、不可压牛顿流体的动力学方程、流固交界面的边界条件和环形柱体域内液体线性晃动的动力学公式出发，基于控制方程的量纲分析法，推导了考虑液体晃动效应的堆本体地震响应动力相似关系。基于上述相似关系建立了堆容器堆内构件和堆容器内自由液面流体域的缩尺模型，通过有限体积法分析堆容器堆内构件原型和缩尺模型中液体的晃动固有频率、晃动波高、压力以及液体晃动对堆容器支承裙的倾覆力矩。结果表明本文动力相似关系具有合理性和准确性，可用于堆本体缩尺模型的抗震试验研究。     

Experimental study on prediction model of wet gas pressure drop across single-orifice plate in horizontal pipes in the low gas phase Froude number region

The pressure drop prediction of wet gas across single-orifice plate in horizontal pipes had been solved satisfactorily under an annular-mist flow in the upstream of orifice plates. However, this pressure drop prediction is still not clearly determined when the upstream is in an intermittent flow or stratified flow, which is corresponding to a region of low Fr_G (gas phase Froude number) in the flow pattern map of wet gases. In this study, the wet gas pressure drop across a single-orifice plate was experimentally investigated in the low Fr_G region. By the experiment, the flow pattern transition in the downstream of single-orifice plates, as well as the effects of Fr_G and Fr_L (liquid phase Froude number) on Φ_G (gas phase multiplier), were determined and compared when the upstream is in the flow pattern transition and the stratified flow region, respectively. Prediction performances were examined on the available pressure drop models. It was found that no model could be capable of jointly predicting the wet gas pressure drop in the low Fr_G region with an acceptable accuracy. With a new method of correlating Fr_G and Fr_L simultaneously, new correlations were proposed for the low Fr_G region. Among which the modified Chisholm model shows the best prediction accuracies, with the prediction deviations of Φ_G being within 7% and 3% when the upstream is in flow pattern transition and stratified flow region, respectively.     

Determination of olaquindox,carbadox and cyadox in animal feeds by ultra-performance liquid chromatography tandem mass spectrometry

Olaquindox, carbadox, and cyadox are chemically synthesised antibacterial and growth-promoting agents for animals. At high doses they may exert mutagenicity and hepatic and adrenal toxicities in animals. Regrettably, these substances are frequently abused or misused when added into animal feeds. Thus, developing a sensitive and reliable method for simultaneous determination of olaquindox, carbadox, and cyadox in different kinds of animal feeds is crucially important for food safety monitoring. In this paper we optimised instrumental conditions, extraction solvents, solid phase extraction cartridges, and pH of the loading solvents on the Oasis HLB cartridge. Under the optimal conditions, mean recoveries ranged from 74.1 to 111%, and intra-day and inter-day variations were lower than 14.6% and 10.8%, respectively. The limits of quantification for olaquindox, carbadox, and cyadox were 0.05 mg kg^?1, 0.10 mg kg^?1, and 0.025 mg kg^?1, respectively. The proposed method uses ultra-performance liquid chromatography tandem mass spectrometry and is sensitive and reliable for the simultaneous determination of olaquindox, carbadox, and cyadox in three kinds of animal feeds (specifically, mixed feed, concentrated feed, and additive premixed feed). This method has good precision, high sensitivity, and good reproducibility, and thus it can be used for convenient and accurate determination of olaquindox, carbadox, and cyadox in different kinds of animal feeds.