ABSTRACTA chiral porous organic polymer (cPOP) was synthesized through nucleophilic substitution polymerization between dichloromaleimide and aromatic amine. This cPOP was used as a new chiral stationary phase (CSP) for gas chromatography (GC) chiral separation. In this work, we first used this cPOP as the CSP for gas chromatography to investigate its ability to separate racemic mixtures, including amino acid derivatives, chiral alcohols, aldehydes, alkanes, ketones, esters, and organic acids. The results showed that the column can effectively separate various racemic mixtures and achieve baseline separation of threonine (Rs = 1.91). Furthermore, the separation mechanism was elucidated by density functional theory (DFT) simulation. Additionally, the cPOP column demonstrated good repeatability and stability. The relative standard deviations (RSDs) for intraday were 0.11%–0.12% (n = 3) for the retention time of n‐butyl glycidyl ether, 0.1%–0.34% (n = 3) for interday, and 2.25%–3.37% (n = 3) for column to column. This work shows that cPOP has good potential as chiral stationary phases in gas chromatography.
Porous Organic Polymers (POPs) have garnered increasing research interest due to their potential to integrate the characteristics of porous materials and polymers. The thiol-yne reaction, a novel "click" reaction confirmed in recent years, is characterized by its simplicity, efficiency, and versatility. There has been no reports on the introduction of dual chiral POP via click chemistry as chromatographic stationary phase. This study employed a thiol-yne click chemistry approach to synthesize a dual chiral porous organic polymer (DC-POP) and successfully prepared the DC-POP-coated capillary column. The enantioselectivity of the novel chiral stationary phase (CSP) was investigated. The results demonstrated that the DC-POP possesses excellent separation performance, capable of resolving various racemic mixtures, including amino acid derivatives, chiral alcohols, ketones, esters, epoxides, and organic acids. The column exhibited good separation capabilities for multiple amino acid derivatives (e.g., Rs = 2.99 for arginine) and the number of theoretical plates was determined to be 3448 plates/m. Interestingly, this column was able to separate racemic mixtures that commercial columns could not, complementing the chiral resolution capabilities of both commercial β-DEX 120 columns and porous organic cage-coated capillary columns. Additionally, the impact of injection frequency on separation performance was evaluated. After multiple injections, the column showed good stability and repeatability, with relative standard deviations (n = 5) for retention time and resolution less than 0.7 % and 6.5 %, respectively. Further investigation was carried out into the effects of temperature on the separation by DC-POP-coated capillary column. This study indicates that the first synthesis of DC-POP via thiol-yne click chemistry, showing its potential as a novel CSP for chiral selector in high-resolution GC enantioseparation.
To investigate the targets and mechanism of Hedysarum Multijugum Maxim (HMM) in treatment of bladder cancer (BC). Based on Traditional Chinese Medicine Systems Pharmacology (TCMSP) and gene databases, active substances and potential targets of HMM were screened, and the HMM-active substances-targets-BC (HATB) regulatory network and PPI network were constructed. Hub targets were screened by Cytoscape. The main active substances and Hub targets were molecularly docked with AutoDock and visualized by PyMOL. 12 Hub targets were screened. Molecular docking showed that active substances mainly acted on MAPK14, MAPK1 and CCND1. The bindings of calycosin to MAPK14, formononetin to MAPK14, and calycosin to CCND1 were stable.
Biosensors, devices capable of detecting biomolecules or bioactive substances, have recently become one of the important tools in the fields of bioanalysis and medical diagnostics. A biosensor is an analytical system composed of biosensitive elements and signal-processing elements used to detect various biological and chemical substances. Biomimetic elements are key to biosensor technology and are the components in a sensor that are responsible for identifying the target analyte. The construction methods and working principles of biosensors based on synthetic biomimetic elements, such as DNAzyme, molecular imprinted polymers and aptamers, and their updated applications in biomedical analysis are summarised. Finally, the technical bottlenecks and future development prospects for biomedical analysis are summarised and discussed.
A novel integrated separation process for boron (B), lithium (Li), and magnesium (Mg) is developed using precipitation and three-liquid-phase extraction (TLPE) methods from salt lake brine with high Mg -Li ratio. Simulated brine is precipitated using (NH 4 ) 2 SO 4 and subsequently extracted through the three-liquid-phase system, which comprises 2-ethyl-1,3-hexanediol (BEPD) dissolved in butyl acetate (BA), polyethylene glycol with average molecular weight of 2000 (PEG2000), and brine. After optimizing the experimental conditions, the process achieves a precipitation of 95.6 % for Mg 2 + and extraction rates of 87.2 % for B 3 + , 73.5 % for Li + , and 91.9 % for Mg 2 + . The separation performance for actual brine demonstrates that the extraction rates of B 3 + , Li + , and Mg 2 + are 84.9, 74.8, and 91.5 %, respectively, which are similar to the results obtained from simulated brine. Moreover, TLPE mechanism is analyzed that B is combined with polyhydroxy compounds in the top phase as H 3 BO 3 , while Li + is extracted by the electrostatic interaction of oxygen atom active groups in the middle phase, and Mg 2 + is remained in the bottom phase due to hydration. Our precipitation and TLPE methods show apparent advantages in achieving integrated separation with high efficiency for B, Li, and Mg in the brine.
Background The metal organic cages (MOCs) are an emerging type of porous material that has attracted considerable research interest due to their unique properties, including good stability and well-defined intrinsic cavities. The chiral MOCs with porous structures have broad application prospects in enantiomeric recognition and separation. However, there are almost no relevant reports on chiral MOCs as chiral stationary phases (CSPs) for enantioseparation by high-performance liquid chromatography (HPLC). Results Here, we report for the first time, the chiral MOCs, MOC-PA was “wrapped” onto the silica gel to create a novel HPLC CSP of chiral MOC-PA@SiO2 through wrapped in net method. There are 24 and 20 chiral compounds or chiral drugs, including alcohols, diols, esters, ketones, alkene, epoxides, ethers, organic acids, phenols and amines, were enantioseparated by vary degrees on MOC-PA@SiO2 packed column under both normal phase (NP) and reversed phase (RP) modes, respectively. Furthermore, compared with commercial Chiralpak AD-H and Chiralcel OD-H columns, the MOC-PA@SiO2 packed column exhibits well chiral separation complementarity to them. It can separate some racemates that unable to be or not to be well separated by the Chiralpak AD-H and Chiralcel OD-H columns. Besides, there are four positional isomers were also well separated by MOC-PA@SiO2 packed column. Significance The effects of temperature and injection volume on separation of MOC-PA@SiO2 packed column were further investigated. This column also exhibited excellent repeatability, stability and column-to-column reproducibility on separation in HPLC. This work indicates that chiral MOCs are a promising class of chiral materials to prepare new CSPs for HPLC enantioseparation.
Bovine serum albumin (BSA) has emerged as a biomarker for mammary gland health and cow quality, being recognized as a significant allergenic protein. In this study, a novel flexible molecular imprinted electrochemical sensor by surface electropolymerization using pyrrole (Py) as functional monomer, which can be better applied to the detection of milk quality marker BSA. Based on computational results, with regard to all polypyrrole (PPy) conformations and amino-acid positions within the protein, the BSA molecule remained firmly embedded into PPy polymers with no biological changes. The molecular imprinted electrochemical sensor displayed a broad linear detection range from 1.0 x 10-4 to 50 ng & sdot;mL- 1 (R2 = 0.995) with a low detection limit (LOD) of 4.5 x 10-2 pg & sdot;mL- 1. Additionally, the sensor was highly selective, reproducible, stable and recoverable, suggesting that it might be utilized for the evaluation of milk quality.
Herein, we report a chiral and porous tubular organic molecular cage (3P-1) that was obtained through a [3+6] imine condensation reaction between ETTBA (4,4 ',4 '',4 '''-(ethene-1,1,2,2-tetrayl)-tetrabenzaldehyde) and (R, R)-CHDA ((R, R)-diaminocyclohexane), as the stationary phase for preparing a 3P-1-coated capillary column by the static coating method. Because the chirality of (R, R)-CHDA was transferred from the point to the chiral face of TPE (tetraphenylethylene) during the formation of the 3P-1 cage, it provides a chiral and porous environment within it. The prepared 3P-1 chiral porous cage is verified by a variety of characterizations. Achiral mixtures, including halogenated benzenes, alkylbenzenes, esters, n-alcohols, n-alkanes, Grob reagent and isomers, have been separated on the 3P-1-coated column. In addition, the separation performance for various racemates, including ethers, esters, alcohols, epoxides, and amino acid derivatives, on the 3P-1-coated column was evaluated. Nine racemates including butyl glycidyl ether, gamma-heptalactone, 2-hexanol, 2,3-butanediol, epichlorohydrin, epibromohydrin, 3-buten-2-ol, dl-threonine, and dl-isoleucine have been resolved on this column, and it showed good chiral resolution capacity for them. The 3P-1-coated column exhibited good enantioseparation complementarity for separating some racemates compared with the beta-DEX 120 commercial column, and it could even separate some racemates that the beta-DEX 120 commercial column could not separate well. Furthermore, the prepared 3P-1-coated column presents good reproducibility after multiple injections of the same analytes and good thermal stability. In summary, all of the studies in this work demonstrate the good application potential of the 3P-1-coated capillary for GC separations. The illustration of a chiral and porous tubular organic molecular cage (3P-1) was obtained through a [3+6] imine condensation reaction that used as the chiral stationary phase for preparing a 3P-1-coated capillary column by the static coating method.
课题组是高校进行科学研究的基本单位,承担着高水平人才培养的重任.课题组实验室是开展科学研究的主要场所,其管理水平决定了成果产出的数量和质量.对课题组实验室管理存在的问题从课题组人员管理、仪器设备管理、试剂材料管理和实验室安全与技术管理四个方面进行了分析,找出问题产生的原因,有针对性地给出了解决问题的对策,对提高高校课题组实验室管理水平具有一定的借鉴与参考.
香紫苏醇作为合成龙涎香的中间体和配制香料的一种重要成分,受到香料领域的大量关注.选取微波辅助法和丙酮-萃取结晶法提取和纯化香紫苏醇发酵液中的香紫苏醇.通过单因素实验和响应面法优化了香紫苏醇的提取工艺,获得最佳提取工艺条件:料液比为1∶25(g/mL),微波温度为59℃,提取时间为9.5 min,在此条件下,菌体的提取率为6.26%.丙酮-萃取结晶法分离纯化提取物得到的香紫苏醇纯度为 94.20%,回收率为 63.56%.整个提取和纯化工艺过程步骤少,操作简单,所用溶剂可循环利用,对环境友好,实验结果可为发酵法生产香紫苏醇的工业化提供参考和技术支撑.
传统的实验室安全培训能在一定程度上提高了学生实验室安全意识和知识水平,但对于实际操作能力的提升还有待加强.借助评价量规对课题组中学生的安全知识水平和实际操作能力进行评估,发现了学生对安全问题了解的不足,也给学生学习安全知识和掌握安全操作提出了要求,促进了学生通过自学和互学等形式提高实验室安全水平,显著提升了学生解决安全问题的能力.因此,评价量规是一个在实验室安全教育与培训中值得推广的有效的办法.
利用网络通信协议传输实验数据是替代光盘刻录的有效方式.通过建立利用SMB网络协议实现数据共享的实验数据中心,将科研设备计算机控制系统与老旧教学计算机相连并接入校园网,实现实验数据的网络传输,方便用户随时随地通过网络查询所需的实验数据.在此基础上进一步探讨了实验数据中心在开放共享平台建设和完善中所起的关键作用.
Herein, a chiral multishelled mesoporous carbon nanospheres (MCNs) with unique spiral multishelled hollow mesoporous chiral structure is synthesized; the MCNs can be used as stationary phases for high-resolution gas chromatography (GC) and have good separation capacity. The successful preparation of MCNs is verified by a variety of characterizations. In addition, the MCNs-coated capillary column shows excellent separation performance for n-alkanes, n-alcohols, aromatic compounds, and esters, and it has a faster analysis time than the HP-5 commercial capillary column. The chromatography separation performance for various isomers and racemates of the MCNs stationary phase was evaluated, and it showed good separation capability for amino acid derivatives. The MCNs-coated capillary column has been demonstrated to present good reproducibility and stability. In summary, all of the chromatography experiments in this work indicate that this new stationary phase of the MCNs has good application potential for GC capillary separation.
为确立微波提取柴胡药渣中柴胡皂苷的最佳工艺,采用响应面实验设计优化了提取过程中的工艺参数.基于单因素实验对工艺参数进行初步筛选,进一步的采用响应面实验建立二阶回归模型,优化了提取时间、提取温度、料液比和甲醇体积百分比4个工艺参数.结果发现:提取温度和提取时间的交互作用、提取温度和甲醇体积百分比的交互作用、提取温度和料液比的交互作用对皂苷提取率的影响较为显著;优化最佳工艺参数提取温度为68℃、料液比为1:59 g/mL、提取时间为30 min、甲醇体积百分比为60%.在该工艺参数下柴胡皂苷提取率最大,达到5.14 mg/g.
College biological laboratory safety is an important part of biological safety. In addition to the safety problems of various reagents and equipment, there are also the protection and waste treatment of various plants, experimental animals, microorganisms and human tissues and organs used in the experiment. In college biological laboratories, the cultivation of independent safety awareness of laboratory personnel is weaker than that of biological enterprises, which leads to two kinds of frequent problem events led by safety protection and waste disposal in college biological laboratories in recent years. Starting from the safety of biological laboratory in Colleges and universities, this paper discusses the laboratory safety protection and waste treatment based on the cultivation of independent safety awareness of laboratory personnel.
Metal organic framework–chiral ionic liquid composites Fe-CIL was first used to construct the chiral sensor, which could be used to chiral recognize tryptophan (Trp) enantiomers based on the DPV peak potential difference (Δ E p ) of l / d -Trp.
多糖检测是在生物工程和中药提取与鉴定等研究中最常用的方法之一.利用蒽酮-硫酸法对灵芝多糖进行检测是实验教学中最通用的方法.本文用酶标仪替代传统分光光度计来分析检测多糖,通过对蒽酮-硫酸法在酶标仪上相关使用参数(试剂比例、温度、时间等)优化,建立了用酶标仪分析灵芝多糖的方法,对方法进行了评价.在灵芝多糖分离实验教学中进行了应用实践,取得了满意的结果.该方法能够高通量检测多糖,缩短实验时间,节省大量的危化品试剂,减少废弃试剂处理量.作为科研新方法与传统实验教学相结合的示范,有助于培养学生的创新思维、提高学生分析和解决问题能力.
The present work describes a faithful strategy of dual-template molecularly imprinted polymers (MIP) to chiral recognize and quantify D-Cystine (D-Cys) and L-Cystine (L-Cys) at ultra-trace level through “vector method.” Briefly, one has to saturate association D-Cys while analyzes L-Cys, and vice versa. Herein, the working electrode, magnetic glassy carbon (MGCE), was initially drop-coated with molybdenum disulfide-ionic liquid (MoS 2 -IL) dispersion liquid for large specific surface area and excellent electrical conductivity. After the working electrode was dried naturally, chitosan (CS) was electrodeposited on. And the strong electrostatic interactions between CS and Fe[(CN) 6 ] 3−/4− could further enhance the electric signal. Next, dual-template MIP dispersion liquid was drop-coated on the working electrode. Moreover, Fe 3 O 4 nano-particles (NPs) was regard as the support skeleton material of dual-template MIP, which could significantly improve the bonding strength with MGCE. Herein, the proposed sensor demonstrated good analytical figures of merits with Differential Pulse Voltammetry (DPV), showing that the LOD of L-Cys and D-Cys were 0.7402 pg ml −1 and 0.6136 pg ml −1 respectively, with linear response ranges from 1 pg ml −1 to 12 pg ml −1 for both enantiomers. Furthermore, the proposed sensor exhibited great potential in chiral recognition and biochemical analysis.
A faithful strategy to significantly improve the enantiorecognition ability of chitosan (CS) is proposed via drop-coating molybdenum disulfide (MoS2)-ionic liquid (IL) nanocomposite. The present work describes a novel, simple, and effective chiral interface based on MoS2-IL/CS nanocomposite which was elaborately integrated to combine the electrical signal amplification and space complexity of MoS2-IL and vast enantiorecognition sites of CS for the electrochemical enantiorecognition of tryptophan (Trp) enantiomers. Differential pulse voltammetry (DPV) was adopted to evaluate the potential differences (Delta EP) between the oxidation peaks of L-Trp and D-Trp. MoS2-IL/CS nanocomposite showed higher chiral recognition ability result from spatial asymmetry of MoS2-IL/CS. Herein, several parameters, such as drop-coated volume and concentration of MoS2-IL, electrodeposited viscosity, time and temperature of CS, detection temperature and pH were optimized in order to obtain a large Delta EP signal between L-Trp and D-Trp, and the Delta EP value can reach 53.3 mV under optimal conditions. Furthermore, different percentages of Trp mixtures and DPV peaks potential were detected with a good linear relationship even in the real sample, which indicated that MoS2-IL/CS chiral interface could effectively quantify the enantiomer excess (ee) of Trp enantiomers in Trp mixtures.