Progress in Synthesis，Detection and Clinical Application of Posaconazole北大核心CSCD

Posaconazole,as the second generation of triazole antifungal drugs,has a wide antifungal spectrum and strong antibacterial activity. It is widely used in clinical practice. However,it has been eight years since its publication before it is approved in China. In order to better understand posaconazole,a first-line drug with great clinical demand, this paper summarizes the pharmacokinetics, pharmacological properties,clinical application and synthetic route of posaconazole in the literature at home and abroad. It is hoped that it can fill the gap in the domestic API market,break the current situation that the API is completely dependent on import,and provide a useful reference for the industrial R & D. © 2022, Science Press (China). All rights reserved.     

Hydrothermal Synthesis of PEG-capped ZnS：Mn2＋ Quantum Dots Nanocomposites

Water-soluble Mn2＋-doped ZnS nanocrystals surface capped with polyethylene glycol（expressed as PEG-ZnS：Mn2＋） were synthesized in aqueous solution with PEG as surface modifier without ligand exchange.The particles were obtained via chemical precipitation method at 100 ℃ with an average diameter of 3 nm and a zinc blende structure.The PEG modified on the surface of PEG-ZnS：Mn2＋ nanocrystals rendered the nanocrystals water soluble and biocompatible.And the PEG-ZnS：Mn2＋ nanocrystals have the potential application in molecular assembly and biological fluorescence analysis.The effects of the Mn2＋ concentration,stabilizer concentration,and synthesis time on the photoluminescence（PL） intensity of ZnS：Mn2＋ QDs were also investigated.     

A Novel Glucose Biosensor Based on Palladium Nanoparticles and Its Application in Detection of Glucose Level in Urine

IntroductionThelevelofglucoseinbloodorurineindicateshyper andhypoglycaemia ,bothofwhichcanresultfromavarietyofendocrinedisorders .1 4 Therapidandreliabledetermi nationofglucoselevelisaroutineprojectinclinicchem istry.Urinesamplesaresaferandmoreconvenientthanbloodones .Meanwhile ,theconcentrationofglucoseinserumiscloselyassociatedwiththatinurine .2 4 Eventhoughglucoseelectrodeshavebeensuccessfullyusedinseruminclinicalapplication ,thequestionstillremainedofhowtodetecttheglucoselevelinurine ,wh…     

银铜双金属/组氨酸功能化石墨烯量子点/石墨烯杂化物的制备及其在电化学法测定黄瓜中毒死蜱、克百威和多菌灵上的应用北大核心CSCD

为了提高金属纳米粒子在石墨烯片上的分散度,通过组氨酸功能化石墨烯量子点(His-GQD)作为桥梁,设计合成银铜双金属/His-GQD/石墨烯杂化物(AgCu/His-GQD/G)。His-GQD通过π-π堆积作用固定到氧化石墨烯上,然后与银离子和铜离子结合形成复合物,最后在氮气保护下热还原获得AgCu/His-GQD/G。形成的杂化物表现出独特的三维结构,且银、铜纳米粒子均匀分散在石墨烯片上。基于该杂化物构建了电化学适配体传感器,适配体与杂化物上的银、铜纳米粒子通过Ag-N和Cu-N键连接而修饰到电极表面上,用于毒死蜱、克百威和多菌灵的测定,表现出高的灵敏度和选择性。毒死蜱、克百威和多菌灵标准曲线的线性范围分别为1.00×10^(-2)~1.00×10^(3)pmol·L^(-1)、1.00×10^(-1)~1.00×10^(4)pmol·L^(-1)和1.00~1.00×10^(6)pmol·L^(-1),检出限(3S/N)分别为3.2×10^(-3)pmol·L^(-1)、2.3×10^(-2)pmol·L^(-1)和2.9×10^(-1)pmol·L^(-1)。该适配体传感器用于黄瓜样品中克百威、毒死蜱和多菌灵的测定,仅检出多菌灵,检出量为1.21 pmol·L^(-1)和1.25 pmol·L^(-1);并按标准加入法进行回收试验,回收率为99.3%~100%。     

Preparation and application of novel polymer nanoparticles in the detection of copper ion and cysteineEI北大核心CSCD

A novel amphiphilic copolymer,dipropenoxystyrene anthracene and acrylic acid copolymer（BASA-AA） was designed and synthesized based on divinyl anthracene. The polymer self-assembled rapidly in water to create polymer nanoparticles（BASA-AA NPs）with a uniform size of 45 nm,no dye leakage,and great brightness（Φ= 36%）. Because of the enormous number of carboxyl groups on the surface of the particles,it can disperse extremely well in water,and can be used for the rapid detection of copper ion and cysteine（Cys）in pure water, with the limit of detection of 45 nmol/L. The fluorescent intensity of the nanoparticles will be greatly reduced after the introduction of copper ion,realizing the detection of copper ion with high selectivity and sensitivity. A composite probe made of BASA-AA NPs and copper ion can detect Cys in the range of 0.1-10 µμmol/L,with the detection limit of 84 nmol/L,due to the high binding capacity of the sulfhydryl group and copper ion. The method is simple and rapid in material synthesis and preparation,and shows high selectivity and sensitivity in pure water. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

基于Au@N-CDs纳米复合材料电化学传感器检测左氧氟沙星北大核心CSCD

本文以富氮生物物质为前驱体合成氮掺杂碳点(N-CDs),调控反应时混合溶液pH值,协同发挥N-CDs还原性和稳定性效应,还原HAuCl_(4)生成并稳定Au纳米粒子(AuNPs),以水浴孵化法制备Au@N-CDs纳米复合材料。基于AuNPs良好电催化能力,N-CDs高比表面积和对左氧氟沙星(LEV)亲合力,提高玻碳电极(GCE)对LEV检测的选择性和灵敏度。在pH=6.0磷酸盐缓冲溶液中,于电位0.4V下富集125s,Au@N-CDs/GCE可在利福平、罗红霉素、红霉素等抗生素共存情况下选择性检测LEV,检出限和线性范围分别为1.0×10^(-6) mol/L和2.5×10^(-6)~1.0×10^(-4) mol/L。该法成功应用于人体尿样中LEV测定,回收率为93.0%~107.4%,相对标准偏差为2.98%。     

分子印迹荧光探针在农药检测中的应用进展北大核心CSCD

分子印迹聚合物由于可特异性地从样品溶液中富集目标物,已被广泛应用于粮食、果蔬等食品以及水、土壤等环境中农药的提取和检测.将分子印迹技术和量子点修饰技术相结合形成的分子印迹荧光探针,可以实现对目标物的高灵敏快速检测.据此,对分子印迹技术的原理、制备方法及应用进行了概述,并进一步阐述了量子点修饰的分子印迹荧光探针在农药检测中的应用和展望.     

金纳米粒子/石墨烯量子点复合修饰电极检测NO_(2)^(-)北大核心CSCD

采用微波加热石墨烯量子点还原HAuCl_(4)的方法,制备金纳米粒子/石墨烯量子点(AuNPs/GQDs)复合物,并将其应用于构建具有高灵敏度的NO_(2)^(-)电化学传感器。由于GQDs大的比表面积和AuNPs良好的导电能力,合成的AuNPs/GQDs复合材料显著提高了NO_(2)^(-)的电化学响应。利用循环伏安法研究NO_(2)^(-)在AuNPs/GQDs修饰电极上的电化学性质,发现在电位1.22 V处出现一个明显的氧化特征峰,其氧化峰电流与NO_(2)^(-)浓度成线性关系,线性范围为1.0×10^(-7)~1.0×10^(-5) mol/L,检测限(S/N=3)为5.0×10^(-8) mol/L。将该方法应用于土壤中NO_(2)^(-)的检测,具有较好的准确度。     

Preparation of Formyl Deoxycholic Acid Modified Fe3O4 Nanoparticles and Their Application for Oxytetracycline Loading北大核心CSCD

Formyldeoxycholic acid modified Fe3O4 nanoparticles（FDCA-MNPs）have been successfully constructed. The structure,morphology and magnetic properties of FDCA-MNPs are characterized by Fourier transform infrared spectroscopy（FT-IR）,transmission electron microscopy（TEM）and vibrating sample magnetometer. Oxytetracycline（OTC）is used as a model drug to evaluate the drug loading and release behaviors of FDCA-MNPs. The maximum loading of OTC is 59. 7 mg/g,and the loading behavior follows Freundlich adsorption balance equations with multilayer adsorption．Furthermore,FDCA-MNPs@OTC shows a higher release rate at pH=9 （11. 8%）than that of pH=7（8. 8%）. The bacteriostatic activities of FDCA-MNPs,OTC,FDCA-MNPs@OTC against E. coli are compared in vitro. The results show that FDCA-MNPs have no inhibition-activity for E. coli, meanwhile,FDCA-MNPs@OTC displays better sterilization ability than OTC at the same concentration. The minimum antibacterial concentration is 3 μg/mL,and the antibacterial rate reaches 97. 8%. It is proved that the synergistic effect of drug carrier and drugs reveals good antibacterial properties and reduce the dosage of antibiotics. © 2022, Science Press (China). All rights reserved.     

Preparation of Oxidized Organosolv Lignin⁃based Hydrophilic Sizing Agent and Its Application in Polypropylene北大核心CSCD

The interfacial compatibility of carbon fiber （CF） reinforced composites is the key factor to determine the comprehensive properties of the composites. The sizing agent plays an indispensable role between carbon fibers and matrix resins. Environmentally friendly hydrophilic sizing agent is is a hot research issue to be solved. In this work,the hydrophilic lignin-based sizing agent and carbon fiber reinforced polypropylene （PP） composites are prepared and studied. The lignin is ozonized to increase the reactive group. The obtained lignin reacts with epoxy group to prepare the oxidized organic solvent lignin based epoxy resin（OLBE）. OLBE reacts with alcohol amine and carboxylic acid to obtain the hydrophilic lignin-based sizing agent. KH550 is further added to balance the hygroscopicity of sizing agent. Finally,an oxidized organic solvent lignin-based hydrophilic sizing agent（OLBEDK）with excellent stability was prepared. The CF treated with 2. 5% solid content OLBEDK was only 3. 0 mg. The ILSS,Flexural strength,Flexural modulus and Impact strength of CF/PP composites are increased by 50. 8%,34. 2%,53. 7% and 127. 8%, respectively,compared with those of CF/PP composites without sizing. This is attributed to the π-π conjugation between the benzene ring of lignin and the carbon six-membered ring of CF,and the physical entanglement between the alkyl chain of KH550 and the molecular chain of PP,which enhances the interfacial interaction between CF and PP effectively. © 2022, Science Press (China). All rights reserved.     

Construction and application of an electrochemical sensor based on graphene-MXene nanocomposites for baicalin detectionEI北大核心CSCD

Redox graphene-MXene(rGO-MXene) nanocomposites were prepared by ion polymerization and used to construct a highly sensitive electrochemical sensor for baicalin(BA) detection. The synergistic effect of rGO and MXene increased the specific surface area and electron transport capacity of the electrode, and significantly enhanced the electrochemical response of BA. The cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behavior of BA on the sensor. Under the optimal conditions, the peak current exhibited a good linear relationship with BA concentration in the range of 0. 05-10 μmol / L, and the limit of detection was as low as 28 nmol / L. The method was applied to analyze traditional Chinese medicine preparations containing baicalin, such as Qingkailing Capsule and Sanhuang Tablets with good accuracy and spiked recovery. The results were highly consistent with those of high performance liquid chromatography, providing a technical means for the rapid and sensitive detection of traditional Chinese medicine preparations. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

Preparation and recognition performance of ratio-fluorescent probe based on sulfadiazine imprinted polymersEI北大核心CSCD

A novel ratio-fluorescent probe based on molecular imprinting polymer ( MIP) for the detection of sulfadiazine was prepared by using nitrogen-doped carbon quantum dots (N-CQDs) as the fluorescence response signal, silica-embedded cadmium telluride quantum dots ( CdTe QDs) as the fluorescence reference signal, sulfadiazine ( SDZ) as template molecule, acrylamide as functional monomer, N, N-methyl bisacrylamide as crosslinking agent and 2,2-Azobisisobutyronitrile as initiator. The results showed that the probe has a core-shell structure and fluorescence sensitive to SDZ, by the characterization of scanning electron microscopy, transmission electron microscopy, and fluorescence spectrophotometer. Under the wavelength of 360 nm, the ratio-fluorescent signal of probe showed a linear response with SDZ concentration in the range of 0-100 μmol / L with the detection limit of 11 nmol / L. Also, the ratio-fluorescent probe was applied to the detection of SDZ with a recovery of 92. 0%-95. 1% and relative standard deviation (RSD) of 3. 6% in real water samples. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

Determination of Pb（II） in environmental water by nano-ceria-graphene modified electrodeEI北大核心CSCD

Nafion solution as a binder,the Gr/CeO2 /Nafion/GCE modified electrode was prepared based on graphene （Gr）-nano cerium oxide （CeO2 ）composite materials. The electrochemical behavior of Pb（II）on the modified electrode was investigated using differential pulse anodic stripping voltammetry （DPASV）. Subsequently,a determination method for Pb（II）was established. The concentrations and ratio of composite materials,buffer solution pH,modification amount,enrichment potential and time were optimized. Under the optimal conditions ,the peak current of Gr/CeO2 /Nafion/GCE showed good linearity in the range of 0.24-48.31 μµmol/L of Pb（II）,and the detection limit was 4.3 nmol/L. Interference experiments showed that the other common anions and cations in water samples caused little interference to Pb（II）detection. Furthermore,the interference of Cu（II）within 10 times is acceptable. The modified electrode was used to the detection of Pb（II） in four complex water samples,and the recovery rates of the spiked assays were from 89.5% to 107.7%. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Construction of ceo2/rgo/gce electrochemical sensor for the determination of histamine in fishEI北大核心CSCD

By preparing nano-CeO2 (CeO2) and reduced graphene oxide (RGO), an electrochemical sensor based on CeO2/RGO composite was constructed for the detection of histamine. The morphology and structure of the composites were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The electrochemical behavior of histamine on the sensor was studied by cyclic voltammetry (CV), and the conditions such as the type proportion and addition amount of the composite scanning rate and buffer pH were optimized. The results showed that the optimal conditions were as follows: The mass ratio was m(CeO2): M(RGO)=1: 0.25, the addition amount of composite material was 10 μL, the scanning rate was 300 mV/s and the pH of buffer solution was 8. A good linear relationship was observed between the peak current and the concentration of histamine in the range of 0.25–100 mg/L with the detection limit of 0.16 mg/L. The CeO2/RGO/GCE electrochemical sensor has been applied to the determination of histamine in fish samples with the spiked recoveries of 98.4% −104%. The method can be used to determine histamine content in fish products. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Recent advancements in analytical methods of phosphodiesterase 5 inhibitors and their metabolitesEI北大核心CSCD

磷酸二酯酶5抑制剂(PDE5i)用于治疗勃起功能障碍和肺动脉高压等疾病。因PDE5i类药物种类繁多,理化性质各异,在体内代谢迅速且具有多种代谢途径,故生物样本检验难度大。本文介绍了PDE5i类药物及其代谢物,总结了生物样本中该类物质的沉淀蛋白法、液-液萃取法、固相萃取法和固相微萃取法等前处理方法,综述了高效液相色谱法、液相色谱质谱联用法、荧光光谱法和电化学分析法等检测方法,展望了PDE5i及其代谢物分析的未来发展方向,以期为PDE5i的药物监测和法庭科学毒物检验提供参考。     

Preparation and application of surface enhanced Raman scattering substrate synthesized from single walled carbon nanotubes and silver nanoparticlesEI北大核心CSCD

By hydrothermal synthesis, silver nanoparticles (AgNPs) arranged on single-walled carbon nanotubes (SWCNTs) uniformly, and a SiO2/CNTs/AgNPs surface enhanced Raman scattering (SERS) substrate with composite open structure was prepared. The synthesized SiO2/CNTs/AgNPs were characterized by transmission electron microscopy (TEM. Using rhodamine 6G(R6G) as the probe molecule, the enhancement factor (EF) was 1.23×108, and the standard deviation was 2.31. Taking the phenol red, a common water pollutant, as the practical sample, the concentration of phenol red in the range of 1×10-4 -1×10-10 mol/L had a great exponential fitting relationship with its Raman signal intensity at 1153 cm-1 and 1441 cm-1, and the correlation coefficient (R2) was 0.99991. The substrate can realize the qualitative and quantitative detection of practical samples. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Effects of trichlorfon on the contents of acetylcholine and choline in fish brain microdialysis samples by UPLC-MS/MS methodEI北大核心CSCD

A combination of microdialysis sampling with ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）was used to quantitatively analyze the effects of organophosphorus pesticides trichlorfon on acetylcholine （ACh） and choline （Ch） in the brain of crucian carp. The mechanism of organophosphorus pesticides poisoning was preliminarily discussed,showing that the ACh content in the brain of fish increased significantly with the increase of the exposure time to trichlorfon,while the Ch content decreased. It indicated that organophosphorus pesticides inhibited the activity of cholinesterase in organisms. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Simultaneous determination of 73 fragrance allergens and 4 pesticides in silicone mosquito repellent products by ultrasonic solvent extraction combined with gas chromatography-tandem mass spectrometryEI北大核心CSCD

以73种致敏性芳香剂与4种农药为目标化合物,建立了硅胶驱蚊手环中致敏性芳香剂与农药同时测定的气相色谱-串联质谱(GC-MS/MS)方法。DB-17MS色谱柱分离,动态多反应监测模式(dMRM),外标法定量。采用阳性样品优化前处理条件,结果显示,以无水乙醇为提取溶剂、密闭控温超声提取可以有效提取硅胶样品中农药与致敏性芳香剂。最佳条件下,77种目标分析物在0.1~100 mg/L范围内线性良好(R^(2)>0.9920),定量限0.02~5.0 mg/kg,回收率66%~120%,相对标准偏差0.2%~9.8%。采用上述方法对14个驱蚊手环样品进行检测,共检出31种目标化合物。该方法可用于硅胶样品中致敏性芳香剂和农药高通量定向筛查。