荧光标记-高效液相色谱测定多肽（PC2～PC6）的研究

基于多肽(Polypeptides PC2~PC6)中富有巯基(-SH)官能团,其与单溴二胺(Monobromobimanes mBBr)能够发生缩合反应,生成具有荧光信号的多肽衍生物;通过优化色谱分离条件,建立了高效液相色谱(荧光检测器)测定多肽的方法;试验中利用质谱鉴定了PCs与mBBr缩合反应的比例关系。结果显示,通过比较PCs标记前后化合物的质谱图,PCs与mBBr反应比例关系为1∶1,稳定性好;高效液相色谱-荧光法测定多肽化合物,五种化合物间分离度较好,出峰时间集中在16.6~22.0min间;PC2,PC3,PC4,PC5和PC6线性相关性系数>0.999 1,方法定量限分别为0.3,0.05,0.3,0.5和0.8 mg·L-1,回收率范围为83.0%~102.0%;重线性较好,RSD<2.0%,该方法实现了多肽类化合物快速、准确定量分析。     

热延迟荧光(TADF)光敏剂的设计合成及其光催化脱卤反应性能研究

以提高光催化效率为目的,设计并合成了一种三咔唑基苯二腈类的热延迟荧光(TADF)光催化剂,建立了在室温下光诱导的芳基卤代物的脱卤反应体系,以TADF为光催化剂,二硫醚为氢转移催化剂,不同的有机卤化物(包括C—Br键和C—Cl键)都可以实现脱卤,且能得到中等至优异的产量.相较于热延迟荧光材料的代表2,4,5,6-四(9H-咔唑-9-基)异酞腈(4CzIPN),设计合成的4-(N,N-二甲氨基)-3,5,6-三(9-咔唑基)邻苯二腈(3Cz DMAPN)具有更高催化效率和专一性.     

层状复合氢氧化物的有机改性方法及应用研究进展

层状复合氢氧化物(LDHs)因其化学组成可调、比表面积大、生物相容性好等特点,目前在环境、能源和生物医药等领域广受关注.然而, LDHs在合成过程中由于其分子内作用力易发生团聚而导致其在基体中的分散不均匀,极大地限制了LDHs在实际中的应用.有机改性是改善LDHs分散性的有效方法,从表面改性和插层改性两个方面综述了近年来LDHs的有机改性方法,并介绍了其在阻燃、吸附、催化、气体阻隔、发光、储能和生物医药材料等领域的应用.最后对改性后LDHs未来的研究方向和应用领域进行了展望.     

钴(Ⅱ)酞菁全氟化策略用于提升非贵金属体系中光催化还原CO2性能(英文)

将CO₂还原成含碳能源或化学品,不仅能够缓解温室气体造成的危害,也是实现“双碳”目标的有效途径.为了有效避免竞争性的产氢反应和克服CO₂的惰性,需要合适的催化剂提高还原产物CO₂的选择性,并促进反应的快速进行.由于以过渡金属配合物为主的分子型催化剂具备已知的清晰结构,且具有丰富多变的氧化还原性质,有助于进行结构优化、分离催化中间体和机理分析,分子型CO₂还原催化剂目前受到了广泛关注.另一方面,利用地壳储量丰富的非贵金属替代珍贵的4d和5d过渡金属来制备分子催化剂有利于降低制备成本,实现大规模应用.因此,设计和优化非贵金属分子催化剂用于光催化CO₂还原是非常有必要的.目前主要的优化方法包括调控电子效应、调控配体共轭程度、设置质子传递中心和设置库仑相互作用等.其中,通过添加给电子/吸电子取代基团来调节配体骨架的电子性质,可以有效调节金属中心的电子密度,从而改善分子催化剂的氧化还原性质.然而,采取该策略可能会导致催化活性和过电位间的此消彼长,限制了催化剂的提升空间.因此,电子效应调控...     

纳米SiC基光催化剂研究进展

Industrialization undoubtedly boosts economic development and improves the standard of living; however, it also leads to some serious problems, including the energy crisis, environmental pollution, and global warming. These problems are associated with or caused by the high carbon dioxide (CO₂) and sulfur dioxide (SO₂) emissions from the burning of fossil fuels such as coal, oil, and gas. Photocatalysis is considered one of the most promising technologies for eliminating these problems because of the possibility of converting CO₂ into hydrocarbon fuels and other valuable chemicals using solar energy, hydrogen (H₂) production from water (H₂O) electrolysis, and degradation of pollutants. Among the various photocatalysts, silicon carbide (SiC) has great potential in the fields of photocatalysis, photoelectrocatalysis, and electrocatalysis because of its good electrical properties and photoelectrochemistry. This review is divided into six sections: introduction, fundamentals of nanostructured SiC, synthesis methods for obtaining nanostructured SiC photocatalysts, strategies for improving the activity of nanostructured SiC photocatalysts, applications of nanostructured SiC photocatalysts, and conclusions and prospects. The fundamentals of nanostructured SiC include its physicochemical characteristics. It possesses a range of unique physical properties, such as extreme hardness, high mechanical stability at high temperatures, a low thermal expansion coefficient, wide bandgap, and superior thermal conductivity. It also possesses exceptional chemical characteristics, such as high oxidation and corrosion resistance. The synthesis methods for obtaining nanostructured SiC have been systematically summarized as follows: Template growth, sol-gel, organic precursor pyrolysis, solvothermal synthesis, arc discharge, carbon thermal reduction, and electrospinning. These synthesis methods require high temperatures, and the reaction mechanism involves SiC formation via the reaction between carbon and silicon oxide. In the section of the review involving the strategies for improving the activity of nanostructured SiC photocatalysts, seven strategies are discussed, viz., element doping, construction of Z-scheme (or S-scheme) systems, supported co-catalysts, visible photosensitization, construction of semiconductor heterojunctions, supported carbon materials, and construction of nanostructures. All of these strategies, except element doping and visible photosensitization, concentrate on enhancing the separation of holes and electrons, while suppressing their recombination, thus improving the photocatalytic performance of the nanostructured SiC photocatalysts. Regarding the element doping and visible photosensitization strategies, element doping can narrow the bandgap of SiC, which generates more holes and electrons to improve photocatalytic activity. On the other hand, the principle of visible photosensitization is that photo-induced electrons move from photosensitizers to the conduction band of SiC to participate in the reaction, thus enhancing the photocatalytic performance. In the section on the applications of nanostructured SiC, photocatalytic H₂ production, pollutant degradation, CO₂ reduction, photoelectrocatalytic, and electrocatalytic applications will be discussed. The mechanism of a photocatalytic reaction requires the SiC photocatalyst to produce photo-induced electrons and holes during irradiation, which participate in the photocatalytic reaction. For example, photo-induced electrons can transform protons into H₂, as well as CO₂ into methane, methanol, or formic acid. Furthermore, photo-induced holes can convert organic waste into H₂O and CO₂. For photoelectrocatalytic and electrocatalytic applications, SiC is used as a catalyst under high temperatures and highly acidic or basic environments because of its remarkable physicochemical characteristics, including low thermal expansion, superior thermal conductivity, and high oxidation and corrosion resistance. The last section of the review will reveal the major obstacles impeding the industrial application of nanostructured SiC photocatalysts, such as insufficient visible absorption, slow reaction kinetics, and hard fabrication, as well as provide some ideas on how to overcome these obstacles.      

Determination of macrolides in livestock excreta by syringe purification coupled with liquid chromatography tandem mass spectrometryEI北大核心CSCD

A method of syringe-dispersive solid-phase extraction combined with ultrahigh performance liquid chromatography with tandem mass spectrometry for the simultanous determination of 10 macrolides in manurebased fertilizers was developed. After extraction with methanol and acetonitrile,the extracts were purified by insyringe dispersion solid-phase extraction in syringes pre-filled with 60 mg PSA and 30 mg C18. The resulted extracts were further separated by a BEH C18 column,detected by multiple reaction monitoring in electrospray positive ion mode,and quantified by matrix-matched external standard method. The results showed that the recoveries of the target compounds ranged from 70% to 110% at three spiked levels（10,30,and 50 μµg/kg）with the relative standard deviations ranged from 1.4% to 12%. The limits of detection and quantification were 0.57 1.75 and 2.77-5.40 μµg/kg,respectively. This method was suitable for the simultaneous determination of residual macrolides in organic fertilizers. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

酸水解-酶水解-UPLC-MS/MS测定特殊医学用途配方食品中多种氨基酸和牛磺酸

利用酸水解与酶水解互补,采用超高效液相色谱-串联质谱法（UPLC-MS/MS）,建立了特殊医学用途配方食品中22种氨基酸和牛磺酸的检测方法。样品经酸水解或酶水解提取,采用6-氨基喹啉基-N-羟基琥珀酰亚胺-氨基甲酸酯（AQC）衍生后,以乙腈-甲酸铵（10 mmol/L）为流动相梯度洗脱,通过AccQTag Ultra C18色谱柱进行分离,三重四极杆质谱电喷雾多反应监测模式检测,内标法定量。结果表明：22种氨基酸和牛磺酸线性关系良好,相关系数均大于0.9956;检出限在0.0028～0.0225 g/100 g之间,定量限在0.0094～0.0751 g/100 g之间。22种氨基酸和牛磺酸的平均加标回收率在90.1%～104.7%之间,相对标准偏差在1.1%～4.3%之间。该方法实现了GB 29922-2013和GB 25596-2010中规定的22种不同性质氨基酸以及牛磺酸成分的水解提取与准确测定,适用于特殊医学用途配方食品中氨基酸和牛磺酸的准确定性、定量分析。     

超高效液相色谱-串联质谱法测定化妆品中61种性激素

建立了一种超高效液相色谱-串联质谱法测定化妆品中61种性激素的方法。水基类、乳液类、膏霜类和凝胶类化妆品经乙腈分散,50%(V/V)乙腈水溶液超声提取;油基类样品经正己烷分散,70%(V/V)乙腈水溶液涡旋提取。采用CORTECS C18(2.1 mm×150 mm, 2.7μm)色谱柱进行分离,选择乙腈、水为流动相进行梯度洗脱,多反应监测(MRM)模式检测,基质外标法定量。结果表明,61种性激素的检出限和定量限分别为0.03～0.31μg/g和0.09～0.92μg/g,在15～150μg/L范围内线性关系良好(相关系数R²>0.99)。选择了5种化妆品基质,在低、中、高3个加标水平下,61种性激素的加标回收率为80.0%～117.7%,相对标准偏差(RSD)为1.5%～14%。该方法可以为化妆品的快速风险筛查和国家标准的制修订提供技术支撑。     

Z型CdIn2S4/ZnSnO3异质结的构筑及其光催化产氢性能

通过高温煅烧ZnSn(OH)₆前驱体制备了双壳中空立方体结构的ZnSnO₃(ZSO),进而采用水热法将CdIn₂S₄(CIS)纳米晶包裹在ZSO表面,成功制备了CdIn₂S₄/ZnSnO₃(CIS/ZSO)异质催化剂。活性产氢实验结果表明,CIS、ZSO物质的量之比为12%时制备的12% CIS/ZSO具有优异的光催化产氢性能,在3 h内产氢量为1 676.48 μmol·g^-1,分别是ZSO和CIS的12倍和8倍。ZSO光催化析氢反应活性的增强归因于CIS/ZSO异质结构的成功构建,异质界面的形成显著提高了光生电子/空穴对的分离效率,降低了其复合率。通过对电荷转移路径的分析,提出了可能的反应机理。     

高效液相色谱-电喷雾检测器法测定香精香料中甜蜜素的含量北大核心CSCD

香精香料是食品添加剂中的一个重要组成部分,由人工调配混合而成,其中含有2种或2种以上的香料,一般由天然提取香料、化学试剂、合成香料、甜味剂等多种成分构成[1]。随着香精香料使用范围的不断扩大,人们对香精香料质量控制等问题的关注度越来越高[2]。目前,为加强食品添加剂的规范生产经营,国家标准GB2760-2014《食品安全国家标准食品添加剂使用标准》对一些易滥用食品添加剂进行了严格的限量规定[3]。