2025年47(1)中英文摘要
时间:2025-01-11      来源:化学试剂

综述与专论

中药多糖药理活性最新研究进展

 

吕嘉璐a,霍燕菊b,张翼*a

(黑龙江中医药大学 a.教育部北药基础与应用研究重点实验室b. 第一临床医学院,黑龙江 哈尔滨  150036)

 

摘要:近年来,中药多糖因较低的毒副作用,多样的药理活性以及广阔的应用前景,成为天然药物开发及应用研究的热点。对近5年的中药多糖研究进行了追踪,汇总整理了中药多糖发挥的抗肿瘤、免疫调节、糖脂代谢、肠道菌群、抗氧化及其他药理活性,并对影响中药多糖药理活性的因素进行了剖析。分析了当前中药多糖研究中存在的局限性,并对未来中药多糖的应用前景进行展望,旨在提高中药材的利用率,明确中药多糖的药理活性,从而加速中药多糖的成果转化及应用推广。

关键词:中药多糖;药理活性;抗肿瘤;免疫调节;肠道代谢稳态调节;作用机制

中图分类号R96              文献标识码A              文章编号0258-3283(2025)01-0001-08

DOI10.13822/j.cnki.hxsj.2024.0293

 

Latest Advancements Research on Pharmacological Activity of Polysaccharides in Chinese Medicine  LV Jia-lua, HUO Yan-jub, ZHANG Yi*a (a.Key Laboratory of Basic and Application Research of Beiyao, 1b.Heilongjiang University of Chinese Medicine, First School of Clinical Medicine, Harbin 150036, China)

Abstract In recent years, polysaccharides in traditional Chinese medicine have become a hot spot in the development and application of natural medicines due to their low toxicity and side effects, diverse pharmacological activities, and broad application prospects. In this study, we tracked the research on polysaccharides in traditional Chinese medicine in recent years, summarized the anti-tumor, immunomodulatory, glucose and lipid metabolism, intestinal microbiota, antioxidant, and other pharmacological activities of traditional Chinese medicine polysaccharides, and analyzed the factors affecting the pharmacological activities of traditional Chinese medicine polysaccharides. This paper analyzed the limitations of the current research on polysaccharides in traditional Chinese medicine and presented  the future application prospects of polysaccharides in traditional Chinese medicine, to achieve three aims: first, to improve the utilization rate of traditional Chinese medicines, second, to clarify the pharmacological activity of traditional Chinese medicine polysaccharides, and third, to accelerate the transformation and application of traditional Chinese medicine polysaccharides.

Key wordstraditional Chinese medicine polysaccharide; pharmacological activity; anti-tumor; immune regulation; regulation of intestinal metabolic homeostasis; mechanism


铜催化的串联环化反应研究进展

 

单系宇1,强泳侨1,2, 何华锋*1

(1. 济宁医学院 药学院,山东 日照  276826

2. 山东第一医科大学(山东省科学院) 药学院(药物研究所),山东 济南  271016)

 

摘要:铜催化的串联环化反应,凭借条件温和、原子经济性高、反应高效受到合成化学研究人员的广泛关注。系统梳理近年来,铜催化的串联环化反应,以便相关领域研究人员更准确、更便捷认识铜催化的串联环化反应,进而开展更深入的拓展。文章依据串联反应中铜催化中心的价态,结合铜盐的参与程度,分别介绍了单一亚铜盐、亚铜盐协同参与、单一二价铜盐催化以及二价铜盐协同参与的串联环化反应。结合绿色化学要求以及铜盐催化反应涉及的配体、反应拓展可能性,指出未来铜催化的串联环化反应的研究热点与方向。

关键词:铜催化; 串联反应; 亚铜盐; 二价铜; 杂环化合物

中图分类号:0621.3        文献标志码:A             文章编号0258-3283(2025)01-0009-08

DOI10.13822/j.cnki.hxsj.2024.0354

 

Advances in Copper-Catalyzed Tandem Cyclization Reaction  SHAN Xi-yu 1, QIANG Yong-qiao 1,2, HE Hua-Feng*1  (1. School of Pharmacy, Jining Medical University, Rizhao China, 276826; 2. School of Pharmaceutical Sciences & Institute of Materia Medica, Shandong First Medical University & Shandong Academy of Medical Sciences, Jinan China, 271016)

Abstract: Tandem cyclization reaction catalyzed by copper had been widely concerned by researchers in synthetic chemistry due to its mild conditions, high atomic economy, and high reaction efficiency. Tandem cyclization reactions catalyzed by copper disclosed in recent years were reviewed, so that more precision and more flexible understanding as well as extensive expansion could be achieved. According to the valence state of the copper catalytic center in the reaction and the participation degree of copper salt, the single cuprous salt, cuprous salt co-participation, single bivalent copper salt catalysis and bivalent copper salt co-participation tandem cyclization reactions were introduced respectively. According to the requirements of green chemistry, ligands involved in copper catalyzed reaction and the possibility of reaction expansion, the research hotspot and direction of copper catalyzed tandem cyclization reaction in the future are proposed.

Key words: Copper-catalyzed; cascade reaction; Cu(I); Cu(II); heterocyclic compound


功能材料

手性金属-有机框架二维材料的液相色谱拆分性能研究

 

王雪萍,高顺秋,李毅洁,杨梅芳,龙怡幸,袁黎明*

(云南师范大学 化学化工学院,云南 昆明  650500)

 

摘要:二维金属-有机框架材(2D-MOFs)具有大比表面积、厚度小、活性位点充分暴露、传质阻力小等优点,将其用作高效液相色谱(HPLC)固定相理论上可以增加色谱柱的塔板数,进而提高其分离效能,在手性分离领域展现出独特的应用价值。将手性分子L-羟基脯氨酸和D-(+)-葡萄糖分别修饰到NH2-Ni/Co MOFsZn-NH2-BDC MOFs两种2D-MOFs上,制备二维手性金属-有机框架纳米片(2D-CMOFs),再将Zn-NH2-BDC-D-(+)-葡萄糖NH2-Ni/Co-L-羟基脯氨酸通过“网包法”固载在硅胶表面制备手性固定相。实验表明:19种手性药物和5种位置异构体被NH2-Ni/Co-L-羟基脯氨酸手性色谱柱拆分开,基线分离了6种手性药物和3种位置异构体;10种手性药物和3种位置异构体被Zn-NH2-BDC-D-(+)-葡萄糖色手性谱柱拆分开;且两个手性柱都具有良好的重复性。

关键词:手性分离;二维手性金属-有机框架材料;手性固定相;高效液相色谱;手性化合物

中图分类号O657. 7          文献标A              文章编号0258-3283202501-0017-09

DOI10.13822/j.cnki.hxsj.2024.0336

 

Resolution Characteristic of Two Chiral Two-Dimensional Metal-Organic Frameworks in Liquid Chromatography WANG Xue-ping, GAO Shun-qiu,LI Yi-jie, YANG Mei-fang, LONG Yi-xing, YUAN Li-ming*(School of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650500, China)

Abstract: Two-dimensional metal-organic frame materials (2D-MOFs) have the advantages of large specific surface area, small thickness, full exposure of active sites, and minimal mass transfer resistance. Their application in high-performance liquid chromatography (HPLC) can theoretically increase the number of column plates and improve its separation efficiency, showing unique application value in the chiral separation field. Two-dimensional chiral metal-organic framework nanosheets (2D-CMOFs) were prepared by modifying the chiral molecules L-hydroxyproline and D-(+) -glucose onto NH2-Ni/Co MOFs and Zn-NH2-BDC MOFs, respectively. The chiral stationary phase was created by applying NH2-Ni/Co-L-hydroxyproline and Zn-NH2-BDC-D-(+)-glucose onto the silica gel surface using the "mesh coating method." The results showed that 19 chiral drugs and 5 site isomers were separated by NH2-Ni/ Co-L-hydroxyproline chiral column, and 6 chiral drugs and 3 site isomers were baseline separated. Ten chiral drugs and three site isomers were separated by Zn-NH2-BDC-D-(+) -glucose-colored chiral spectrum. Both chiral columns have good repeatability.

Key words: chiral separation; high-performance liquid chromatography; two-dimensional metal-organic frameworks; chiral stationary phase ;chiral compounds

 

 

基于柔性苯二乙酸CM6@Zn-MOF纳米材料的构筑和光电性能研究

 

李鹏云1, 张军1, 孙朋涛1, 张钢强1, 马雅菲2,张美丽*2

(1. 新疆宣力环保能源股份有限公司,新疆维吾尔自治区 哈密  9630002. 延安大学化学与化工学院,陕西 延安  716000

 

摘要:金属有机框架 (Metal-organic frameworks,简称MOFs) 作为有效能量转移的供体,在人工光采集材料领域中已引起许多专家的关注。特别是二维 MOFs纳米片,因每个活性位点暴露在外易靠近受体,可以有效地将内部能量转移给外部受体,具有更为非凡的光电性能。在本研究中,选用柔性的1,2-苯二乙酸 (H2opda) 和刚性的3,5-(三氮唑)吡啶 (btyp) 作为有机配体,合成了一种新型的二维配位聚合物[Zn3(btyp)2(opda)3(H2O)3]·(btyp)(H2O)3(Zn-MOF)晶体属于三斜晶系、P-1空间群。该晶体结构中,反式opda配体的2个羧基均以双齿螯合模式与ZnII)离子配位,形成一维无限链;btyp配体桥链支撑相邻一维链,构成二维网面;通过opda羧基O结晶H2O之间多个O―H···O的相互作用形成三维超分子网络结构。Zn-MOF具有完整的循环伏安曲线(还原、氧化电位分别为-0.290.05 V),良好的扫描速率。使用超声粉碎法将Zn-MOF层状结构剥离形成二维纳米片,香豆素6 (CM6) 形成CM6@Zn-MOF纳米材料,荧光从蓝光向绿光移动,将光收集范围从紫外光扩展到可见光,加之良好的电化学循环伏安性能(还原、氧化电位分别为-0.210.08 V),有望成为光电应用新材料。

关键词: 水热合成;苯二乙酸;香豆6;晶体结构;掺杂材料;光电性能

中图分类号O641              文献标A              文章编号0258-3283202501-0026-07

DOI10.13822/j.cnki.hxsj.2024.0362

 

Construction and Photoelectric Properties of CM6@Zn-MOF Nanophase Materials Based on Flexible Phenyldiacetate LI Peng-yun1, ZHANG Jun1, SUN Peng-tao1, ZHANG Gang-qiang1, MA Ya-fei2, ZHANG Mei-li*2 (1.Xinjiang Shinning Environmental Protection Energy Co., LTD., Hami 963000, China; 3.College of Chemistry and Chemical Engineering, Yanan University, Yanan 716000, China)

Abstract: Metal-organic frameworks (MOFs), as the donors of efficient energy transfer, have attracted the attention of many experts in the field of artificial light-harvesting materials. In particular, the two-dimensional MOFs nanoplates have more remarkable photoelectric properties because each active site can be easily accessible to the receptor when exposed to the outside, thus effectively transferring the internal energy to the external receptor. In this study, flexible 1,2-phenyldiacetic acid (H2opda) and rigid 3,5-bis (triazole) pyridine (btyp) were selected as organic ligands, a novel coordination polymer [Zn3(btyp)2(opda)3(H2O)3]·(btyp)(H2O) (Zn-MOF) was synthesized, which belonged to triclinic crystal system and P-1 space group. In the crystal structure, the two carboxyl groups of trans-opda ligand form one-dimensional infinite chain with Zn (II) ion by double-tooth chelating coordination; btyp ligands support adjacent one-dimensional chains to form two-dimensional network surface; the three-dimensional supramolecular network structure was formed by the interaction of O―H···O between opda and H2O. Zn-MOF had a complete cyclic voltammetric curve (reduction and oxidation potentials are -0.29 and 0.05 V, respectively), and a good scanning rate. The layered structure of Zn-MOF was peeled off to form two-dimensional nanomaterials by ultrasonic comminution and then doped with coumarin 6(CM6) to form CM6@ZN-MOF nanomaterials. The fluorescence moved from blue to green light, and expanded the light collection range from ultraviolet to visible light. Combined with the good electrochemical cyclic voltammetry performance (reduction and oxidation potentials are -0.21 and 0.08 V, respectively), CM6@Zn-MOF is expected to become a new material for photoelectric applications.

Key words: hydro-thermal synthesis; benzodiacetic acid; coumarin 6; crystal structure; mixed materials; photoelectric properties


多种金属有机框架材料的荧光淬灭-恢复性能研究

 

徐奥,韦宇新,施润呈,孙璇*

(湖北中医药大学 基础医学院,湖北 武汉  430056)

 

摘要:金属有机框架(Metal-organic frameworks, MOFs)作为一种新型多孔晶体材料受到广泛关注,旨在研究其作为生物传感原件中的荧光淬灭-恢复性能。ZIF-8MIL-101(Fe)MIL-101(Cr)UIO-662D-pMOFs 5MOFs材料分别采用溶剂热法进行化学合成,然后分别与荧光探针、互补DNA孵育研究其荧光强度变化,并测定反应液在485 nm激发波长下的荧光强度值。ZIF-8MIL-101(Fe)MIL-101(Cr) 几乎无荧光淬灭-恢复活性,2D-pMOFs具有一定的荧光淬灭-恢复效率,UIO-66的荧光淬灭-恢复效率最强。UIO-66的荧光淬灭特性源于金属离子锆的光诱导电子转移效应;而荧光恢复能力来自其结构上的多孔性。UIO-66通过对DNA的吸附/解吸实现DNA探针的荧光淬灭/恢复,在生物传感领域显示出巨大的应用潜力。

关键词:金属有机框架 (MOFs);荧光淬灭;荧光恢复;荧光探针;纳米材料

中图分类号O65              文献标识码A              文章编号0258-3283202501-0033-06

DOI10.13822/j.cnki.hxsj.2024.0407

 

Study of Fluorescence Quenching-Recovery Properties of a Variety of Metal-Organic Framework Materials  XU Ao , WEI Yu-xin , SHI Run-cheng , SUN Xuan * (School of Basic Medical Sciences, Hubei University of Chinese Medicine, Hubei 430056,China) 

Abstract Metal-Organic Frameworks (MOFs) has attracted widespread attention as a new type of porous crystal material. The aim of this study is to investigate its fluorescence quenching-recovery performance as a biosensor. ZIF-8, MIL-101(Fe), MIL-101(Cr), UIO-66, and 2D-pMOFs were synthesized by solvothermal method, and then incubated them with fluorescent probes and complementary DNA to study their fluorescence intensity changes. ZIF-8, MIL-101(Fe) and MIL-101(Cr) had almost no fluorescence quenching-recovery activity, 2D-pMOFs had certain fluorescence quenching-recovery efficiency, and UIO-66 had the strongest fluorescence quenching-recovery efficiency. The fluorescence quenching properties of UIO-66 were derived from the photoinduced electron transfer (PET) effect of zirconium metal ions. The fluorescence recovery ability comed from its structural porosity. UIO-66 realized fluorescence quenching/recovery of DNA probes through adsorption/desorption of DNA, and showed great application potential in the field of biosensor.

Key wordsmetal-organic frameworks (MOFs); fluorescence quenching; fluorescence recovery; fluorescent probe; nanomaterials


球形花状多孔碳材料制备及应用

 

刘亚东,白广梅,邱文革*

(北京工业大学 材料科学与工程学院,北京  100124

 

摘要:采用老化处理与水热碳化结合的策略,以葡萄糖为碳源,成功制备了球形花状多孔碳材料,相应Pd(OH)2/C催化剂在笼形底物的氢解脱苄反应中显示出优异的催化活性。具体研究了MgCl2/Na2CO3物质的量比、葡萄糖浓度和老化处理对碳材料形貌的影响,确定了球形花状多孔碳材料的较佳制备条件。通过扫描电镜、粉末X射线衍射和氮气吸/脱附测试表征了原位自生模板剂和多孔碳材料的形貌、晶相结构及比表面积和孔径分布。发现将MgCl2Na2CO3在常温下混合,首先生成的是棒状碳酸镁,经过80℃老化处理后,转变为球形花状碱式碳酸镁,它是葡萄糖水热碳化的模板剂。

关键词:多孔碳材料;水热合成;原位自生模板法;老化处理;氢解脱苄

中图分类号TQ152              文献标A            文章编号0258-3283202501-0039-06

DOI10.13822/j.cnki.hxsj.2024.0363

 

Preparation and Application of Spherical Flower-like Porous Carbon Material LIU Ya-dong, BAI Guang-mei, QIU Wen-ge* (College of Materials Science and Engineering, Beijing University of Technology, Beijing 100124, China)

AbstractPorous carbon material with a spherical, flower-like structure was successfully synthesized using a combination approach involving aging treatment and hydrothermal carbonization, with glucose serving as the carbon source.  The corresponding Pd(OH)2/C catalyst showed high activity in the hydrogenolytic debenzylation of a cage substrate. The effects of the mole ratio of MgCl2/Na2CO3, glucose concentration, and aging treatment on the morphology of porous carbon material were studied, and the optimum preparation conditions were determined. The morphology, crystalline structure, specific surface area, and pore size distribution of the resulting porous carbon material were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and nitrogen adsorption and desorption test. It was found that rod-shaped magnesium carbonate formed firstly when MgCl2 and Na2CO3 were mixed at room temperature, which transformed to spherical flower-like basic magnesium carbonate after aging treatment at 80 , templating the glucose hydrothermal carbonization.

Key words: porous carbon material; hydrothermal synthesis; in situ self-generating template strategy; aging treatmenthydrogenolytic debenzylation


硬碳负极材料储钠性能的影响因素分析

 

杨耀1,陈平2,3,施志聪*1

1. 广东工业大学 材料与能源学院 新能源材料与器件系,广东 广州  510000

2. 深圳市电科电源股份有限公司,广东 深圳  518000

3. 衡阳电科电源有限公司,湖南 衡阳  421000

 

摘要:以木质素磺酸钠和酚醛树脂为前驱体,采用喷雾干燥和油浴干燥两种方法制备硬碳前驱体,前驱体在预氧化、碳化及清洗步骤后得到硬碳材料。通过扫描电子显微镜、X射线衍射、氮气吸附/脱附测试和拉曼光谱等方法探究采用不同制备方法合成的硬碳材料在结构形貌和物相上的差别。并通过电化学测试分析所制备的硬碳材料的电化学性能。结果表明,采用喷雾干燥法合成的硬碳前驱体制备的硬碳材料具有更稳定的球形结构和较小的比表面积。作为钠离子电池负极材料,这种硬碳材料在电池中展现出更高的首次库伦效率,并且具有更稳定的循环性能。

关键词:硬碳;钠离子电池;负极材料;喷雾干燥;油浴干燥

中图分类号:TM911      文献标识码:A      文章编号:0258-3283202501-0045-06

DOI10.13822/j.cnki.hxsj.2024.0308

 

Analysis of Factors Affecting the Sodium Storage Performance of Hard Carbon Anode Materials  YANG Yao1, CHEN Ping2,3, SHI Zhi-cong*11. School of Materials and Energy, Guangdong University of Technology, Guangzhou 510000, China2. BST Power (Shenzhen) Limited, Shenzhen 518000, China3. Hengyang BST Power Limited, Hengyang 421000, China)   

Abstract: The sodium lignosulfonate and phenolic resin are used as the precursors to prepare hard carbon precursors through spray drying or oil bath drying methods. The final hard carbon material is obtained after pre-oxidation, carbonization, and cleaning steps. Scanning electron microscopy, X-ray diffraction, nitrogen adsorption/desorption test, and Raman spectroscopy are used to investigate the differences in the structure and phase of the hard carbon materials synthesized by different preparation methods. The electrochemical performance of the materials prepared by the two methods is analyzed through electrochemical tests. The results indicate that the hard carbon material prepared from hard carbon precursor synthesized by the spray drying method exhibits a more stable spherical structure and smaller specific surface area. As an anode material for sodium ion batteries, this hard carbon material demonstrates higher initial Coulombic efficiency in the battery and better cycling stability.

Key words: hard carbon ; sodium ions batteries ; anode material; spray drying; oil bath drying


芹菜生物碳及其复合材料的制备、表征和燃烧催化性能研究

张引莉高丰琴,刘洋,李午戊,齐珂琪,范广*

(咸阳师范学院 化学与化工学院, 陕西 咸阳 712000)

 

摘要:碳材料因其独特的电子结构和高比表面积,能够有效地催化含能材料的分解反应,从而提高能量释放的效率和速率。以芹菜为原料通过热解方式制备了生物碳及其复合物:QC-760QC@Fe-760QC@Bi-760QC@Fe0-760QC@Fe-450QC@Bi-450。首先,利用IRXRDSEMBET等对其做了相关表征,结果表明,相对于芹菜粉末,QC-760的比表面积增大了17倍。其次,探究了芹菜生物碳及其复合物对高氯酸铵(AP)、奥克托金(HMX)黑索金(RDX)的热分解行为的影响,结果表明,生物碳及其复合物均对APRDXHMX的分解过程影响较大;其中,QC@Bi-450AP催化性能最佳,放热量达到3344 J/gQC-760RDX的催化性能最好,使其放热峰温提前了41 °C,放热量增加了713 J/gQC@Fe0-760使HMX分解峰温提前了82 °C最后,测试了样品对罗丹明B的吸附性能,发现搅拌时间为80 min,样品质量为2 mg/mL,罗丹明B浓度为350 mg/L时,QC-760吸附性能最好。

关键词:生物碳;催化;含能材料;芹菜;热分解

中图分类号O613.71               文献标识码: A         文章编号0258-3283202501-0051-10

DOI10.13822/j.cnki.hxsj.2024.0403

 

Preparation, Characterization and Combustion Catalytic Performance of Celery Biochar and Its Composite Materials ZHANG Yin-li, GAO Feng-qin, LIU Yang, LI Wu-wu, QI Ke-qi, Fan Guang* (College of Chemistry and Chemical Engineering, Xianyang Normal University,Xianyang, Shaanxi 712000, China)

Abstract: Carbon materials, due to their unique electronic structure and high specific surface area, can effectively catalyze the decomposition reactions of energetic materials, thereby improving the efficiency and rate of energy release. In this paper, biological carbon and its composites, QC-760, QC@Fe-760, QC@Bi-760, QC@Fe0-760, QC@Fe-450, and QC@Bi-450, were prepared from celery as raw material through pyrolysis. Firstly, characterization was performed using IR, XRD, SEM, and BET, and the results showed that the specific surface area of QC-760 increased by 17 times compared to celery powder. Secondly, the effects of celery biochar and its composites on the thermal decomposition behavior of ammonium perchlorate (AP), octogen (HMX), and cyclotrimethylenetrinitramine (RDX) were investigated. The results indicated that the biochar and its composites had a significant impact on the decomposition process of AP, RDX, and HMX; among them, QC@Bi-450 had the best catalytic performance for AP, with an exothermic heat reaching 3344 J/g; QC-760 had the best catalytic performance for RDX, advancing its exothermic peak temperature by 41 °C and increasing the exothermic heat by 713 J/g; QC@Fe0-760 advanced the decomposition peak temperature of HMX by 82 °C. Finally, the adsorption performance of the samples on Rhodamine B was tested, and it was found that when the stirring time was 80 minutes, the sample mass was 2 mg per milliliter, and the Rhodamine B concentration was 350 mg/L, QC-760 had the best adsorption performance.

Key words: biochar; catalysis; energetic material; celery; thermolysis


分离提取技术

从柚子落果中提取柚皮苷的杂质谱研究

 

张丽,唐官美,韦媛,卢振鸿,韩方方,张雪晴,郭志勇*

(三峡大学 a.生物与制药学院,b. 天然产物研究与利用湖北省重点实验室,湖北 宜昌  443002)

 

摘要:柚皮苷是一种具有广泛用途的二氢类化合物,为建立基于碱提酸沉柚皮苷提取工艺的质量标准提供物质基础。通过反复重结晶,正向柱层析,制备液相及半制备液相等方法分离纯化,经NMR,圆二色谱等手段鉴定结构从微量杂质中分离鉴定12个杂质,包括4个香豆素类化合物,1个柠檬苦素类化合物,1个简单苯甲酸衍生物和6个黄酮类衍生物,分别为佛手酚 (1)7-Hydroxy-1-benzopiran-2-one (2)Marmin (3)Protocatechuic acid (4)8-(6,7-dihydroxy- 3,7-dimethyloct -1-en-3-yl)-5-hydroxy-6,7-furocoumarin (5)Obacunone (6), 柚皮素 (7)7,4' -Dihydroxyflavone (8), Rhoifolin (9)Vicenin (10)Neoeriocitrin (11)2S-Neoeriocitrin (12)化合物5为首次从柚的果实中分离得到,为建立碱提酸沉工艺提取柚皮苷的质量标准建立提供物质基础。

关键词:柚皮苷;碱提酸沉提取工艺;香豆素;黄酮类化合物;杂质

中图分类号O65              文献标A              文章编号0258-3283 (2025)01-0061-06

DOI10.13822/j.cnki.hxsj.2024.0288

 

Impurities Spectra of Naringin Products from the Abscission Fruits of Citrus Maxima (Burm.) Merr  ZHANG Li, TANG Guan-mei, WEI Yuan, LU Zhen-hong, HAN Fang-fang, ZHANG Xue-qing, GUO Zhi-yong* (a. College of Biological and Pharmaceutical Sciences, b. HuBei Key Laboratory of Natural Products Research and Development, China Three Gorges University, Yichang 443002,China) 

AbstractNaringin is a kind of flavonoid with multiform usages. The impurities were isolated and identified from the alkali extraction and acid precipitation process of naringin. Repeated recrystallization, column chromatography, preparative and semipreparative HPLC was employed for isolation and purification. Then the purified impurities were identified by NMR and CD spectra. The twelve impurities were obtained and determined as Bergaptol (1), 7-Hydroxy-1-benzopiran-2-one (2), Marmin (3), Protocatechuic acid (4), 8-(6,7-dihydroxy-3,7-dimethyloct-1-en-3-yl)-5-hydroxy-6,7-furocoumarin (5), Obacunone (6), Naringin (7), 7,4' -Dihydroxyflavone (8), Rhoifolin (9), Vicenin (10), Neoeriocitrin (11) and 2S-Neoeriocitrin (12). The above twelve impurities will help to establish quality control standards of naringin based on alkali extraction and acid precipitation process.

Key wordsnaringinalkali extraction and acid precipitation processcoumarinsflavonoidsimpurities


化学品与环境

同位素内标稀释-UPLC-MS/MS同时测定生活饮用水中5种消毒副产物和高氯酸盐

 

侯婧,刘双德*

(青海省疾病预防控制中心,青海 西宁  810000

 

摘要:利用同位素稀释技术建立一种可同时测定生活饮用水中二氯乙酸、三氯乙酸、氯酸盐、亚氯酸盐和溴酸盐5种消毒副产物,以及高氯酸盐的超高效液相色谱串联质谱(ID-UPLC-MS/MS)检测方法。样品过膜后加入同位素内标,采用Torus DEA色谱柱(100 mm×2.1 mm1.7 μm)分离,以0.5%氨水-1 mmol/L乙酸铵和乙腈为流动相洗脱,多反应监测(MRM)负模式(ESI-)测定,内标法定量。6种化合物线性相关系数r均大于0.990,检出限为1.5~2.1 μg/L,定量限为5.0~7.0 μg/L,应用该方法对399份水样进行测定,检出率为16.04%。该方法采用同位素内标稀释直接进样,分析速度快,灵敏度高,数据准确适用于饮用水国家标准(GB/T 5750.5-2023GB/T 5750.10-2023)检测限值的要求。

关键词:生活饮用水;超高效液相色谱串联质谱法;消毒副产物;高氯酸盐;Torus DEA色谱柱;同位素内标稀释

中图分类号:O657.63          文献标志码:A          文章编号:0258-3283202501-0067-07

DOI10.13822/j.cnki.hxsj.2024.0335

 

Simultaneous Determination of Five Disinfection Byproducts and Perchlorate in Drinking Water by Isotope Internal Standard Dilution UPLC-MS/MS Method HOU Jing, LIU Shuang-de*Qinghai Center for Disease Prevention and Control, Xining 810000, China

Abstract: An isotope dilution technique coupled with ultra-performance liquid chromatography-tandem mass spectrometry (ID-UPLC-MS/MS) method was established for simultaneous determination of disinfection byproducts such as dichloroacetic acid, trichloroacetic acid, chlorate, chlorite, bromate, and perchlorate in drinking water. The samples were separated by Torus DEA column (100 mm×2.1 mm, 1.7 μm), eluted with 0.5% ammonia-1 mmol/L ammonium acetate and acetonitrile as mobile phases, determined by multiple reaction monitoring (MRM) negative mode (ESI-), and quantified by internal standard method. The linear correlation coefficients for all six compounds were greater than 0.990. The detection limits ranged from 1.5 to 2.1 μg/L, and the quantitation limits ranged from 5.0~7.0 μg/L. The detection rate was 16.04% in 399 water samples. The method involves direct injection of samples using isotope internal standard dilution, resulting in fast analysis speed, high sensitivity, and accurate data. This method is suitable for detecting compounds within the limits set by the drinking water national standards (GB/T 5750.5-2023 and GB/T 5750.10-2023).

Key words: drinking water; ultra performance liquid chromatography-tandem mass spectrometry; disinfection byproducts; perchlorate; torus DEA column; isotope internal standard dilution


加压流体萃取-改进QuEChERS -气相色谱质谱法测定土壤和沉积物中4种新污染物的含量

 

蒋建军1,刘丽*1,蒋家贵1,罗宇2,高帅鹏2

1.广电计量检测(湖南)有限公司,湖南 长沙  4100002.广电计量检测集团股份有限公司,广东 广州  510656

 

摘要:建立了加压流体萃取-改进QuEChERS-气相色谱质谱法测定土壤和沉积物中4种新污染物4-壬基酚2,4-三氯杀螨醇、三氯杀螨醇1,2,5,6,9,10-六溴环十二烷)的方法。取10 g土壤或沉积物样品,以V(正己烷):V(丙酮)=1:1为萃取溶剂,设定萃取温度100℃,静态萃取时间2 min,静态萃取2次,萃取液经无水硫酸钠脱水浓缩,20 mg N-丙基乙二胺(PSA10 mg还原氧化石墨烯净化,涡旋、离心定容,以DB-5MS毛细管色谱柱(30m×0.25µm×0.25mm)分离,结合气相色谱质谱仪同位素内标法进行定性定量检测。结果表明:4种新污染物4-壬基酚2,4-三氯杀螨醇、三氯杀螨醇1,2,5,6,9,10-六溴环十二烷)在质量浓度0.1~1.0 mg/L范围内线性关系良好,相关系数(r)均0.998,对土壤和沉积物不同类型样品的检出限分别为0.8~2.0 μg/kg1.2~2.4 μg/kg,定量限分别为3.2~8.0 μg/kg4.8~9.6 μg/kg。在1050100 μg/kg不同浓度加标水平下,土壤样品的平均加标回收率为83.9%~100.2%相对标准偏差(RSD2.1%~5.0%n=6);沉积物样品的平均加标回收率为72.7%~95.4%相对标准偏差(RSD2.8%~6.8%n=6)。方法应用于某农药厂周边采集的土壤和沉积物样品分析,均有不同浓度的三氯杀螨醇、4-壬基酚和1,2,5,6,9,10-六溴环十二烷检出,检出率为14.1%

关键词:新污染物;土壤;沉积物;加压流体萃取QuEChERS;气相色谱质谱联用

中图分类号:O65         文献标志码:A          文章编号:0258-3283202501-0074-06

DOI10.13822/j.cnki.hxsj.2024.0295

 

Detection of Four New Pollutants in Soil and Sediment by Accelerated Solvent Extraction Modified QuEChERS-Gas Chromatography-Mass Spectrometry  JIANG Jian-jun1, LIU Li*1, JIANG Jia-gui1, LUO Yu2, GAO Shuai-peng2 1.GRG Metrology & testHunanCo, Ltd., Changsha 410000, China; 2. GRG Metrology & test Group Co, Ltd., Guangzhou 510656, China)

Abstract: A method was established for the determination of four new pollutants (4-Nonylphenol, 2,4-Trichlorothiramate, Trichlorothiramate, 1,2,5,6,9,10-Hexabromocyclododecane) in soil and sediment using ASE extraction-Modified QuEChERS purification-GCMS. Ten grams of soil or sediment samples were extracted with a mixture of n-hexane and acetone (1:1, v/v) as the extraction solvent. The extraction was performed at 100°C for 2 minutes with two static extractions. The extract was dehydrated with anhydrous sodium sulfate, purified with 20 mg of N-propylethylenediamine (PSA) and 10 mg of reduced graphene oxide, and then vortexed, centrifuged, and made up to a constant volume. The separation was achieved on a DB-5MS column (30m×0.25µm×0.25mm), and the qualitative and quantitative analysis was performed using gas chromatography-mass spectrometry with an electron impact ionization source (EI) and selected ion monitoring (SIM) mode with the internal standard method. The results showed that the four new pollutants (4-Nonylphenol, 2,4-Trichlorothiramate, Trichlorothiramate, 1,2,5,6,9,10-Hexabromocyclododecane) showed good linearity within the mass concentration range of 0.1~1.0 mg/L, with correlation coefficients (r) all greater than 0.998. The detection limits for soil and sediment samples were 0.8~2.0 μg/kg and 1.2~2.4 μg/kg, respectively. The limits of quantitation were 3.2~8.0 μg/kg and 4.8~9.6 μg/kg, respectively. The average recoveries of soil sample were 83.9%~100.2%, and relative standard deviations(RSDs) were 2.1%~5.0%(n=6) under the standard recovery test at different levels of 10, 50, and 100 μg/kg. The average recoveries of the sediment sample were 72.7%~95.4%, and the relative standard deviation (RSDs) was 2.8%~6.8%(n=6). The method was applied to analyze soil and sediment samples collected around a pesticide factory, and three pesticides, namely trichlorfon, 4-nonylphenol, and 1,2,5,6,9,10-hexabromocyclododecane, were detected at different concentrations, with a detection rate of 14.1%.

Key words: new pollutants; soil ; sediment; accelerated solvent extraction; QuEChERS; GC-MS

 

分析与测试

上海白玉兰花香和鲜花精油挥发性成分的GC-MS分析研究 

 

黄积武1,郭思妤1,王慧敏2,周博文1,王昊阳1,郭寅龙1,刘文*1

(1. 中国科学院上海有机化学研究所 a. 生命过程小分子调控全国重点实验室,b. 分析测试中心,上海  2000322. 上海社会科学院应用经济研究所,上海  200020)

 

摘要:为了比较上海白玉兰花香和白玉兰鲜花精油的成分差异,采用顶空气质联用技术(HS-GC-MS)或气相色谱-质谱联用技术(GC-MS)进行挥发性成分的分析。结果表明,从白玉兰花香和白玉兰鲜花精油中共鉴定出44种成分,相同成分10种;白玉兰花香中共检测出26种成分,相对含量占其总量的96.29%,其主要成分为桉叶油醇(26.73%)、桧烯(23.29%)β-蒎烯(18.77%)β-月桂烯(12.22%)α-蒎烯(6.83%);白玉兰鲜花精油中共检测出28种化学成分,相对含量占其总量的79.46%,主要成分包括苯乙醇(35.48%)、桉叶油醇(10.09%)α-松油醇(9.12%)、柳杉二醇(5.69%)4-松油醇(5.52%)。白玉兰花香和白玉兰鲜花精油成分在类别及相对含量上均有所差异,这为白玉兰资源的合理开发利用提供了理论依据。

关键词:白玉兰;花香;精油;挥发性成分;GC-MS

中图分类号O65              文献标A              文章编号0258-3283202501-0080-06

DOI10.13822/j.cnki.hxsj.2024.0383

 

GC-MS Analysis of Volatile Components in Shanghai Yulania denudate Floral Fragrance and Fresh Flower Essential Oil  HUANG Ji-wu1, GUO Si-yu1, WANG Hui-min2, ZHOU Bo-wen1, WANG Hao-yang1, GUO Yin-long1, LIU Wen*1 (1a. State Key Labratory of Chemical Biology, 1b. Analyses and Testing Center, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032, China; 2. Institute of Applied Economics, Shanghai Academy of Social Sciences, Shanghai 200020, China) 

AbstractTo assess the differences in composition between the fragrance of Shanghai Yulania denudate fresh flowers and the essential oil extracted from fresh Y. denudate flowers, volatile constituents were analyzed by using headspace gas chromatography-mass spectrometry (HS-GC-MS) or gas chromatography-mass spectrometry (GC-MS). The results revealed a total of 44 identified compounds from both fragrance and essential oil, with 10 compounds common to both. The fragrance exhibited 26 components, accounting for 96.29% of the total, characterized predominantly by eucalyptol (26.73%), sabinen (23.29%), β-pinene (18.77%), β-myrcene (12.22%) and α-pinene (6.83%). The fresh flower essential oil contained 28 chemical constituents, comprising 79.46% of the total, with major components including phenylethanol (35.48%), eucalyptol (10.09%), α-terpineol (9.12%), cryptomeridiol (5.69%) and 4-terpineol (5.52%). Differences in the composition and relative proportions of components between the fragrance and essential oil of Y. denudate provide a scientific basis for the rational exploitation of this resource.

Key wordsYulania denudate; floral fragrance; essential oils; volatile components; GC-MS


固相萃取-超高效液相色谱串联质谱法测定猪肉中9种氨基糖苷类抗生素残留

 

周寒琳1,郭杭婷1,张虹*1,陈新旺*2,韩永和1,张勇1,贲玉婕3

1. 福建师范大学 a.环境与资源学院、碳中和现代产业学院,b.福建省污染控制与资源循环利用重点实验室,福建 福州  3501172. 福建医科大学附属协和医院 呼吸与危重症医学科,福建 福州  3500013. 宁波东方理工大学(暂名),浙江 宁波  315200)

 

摘要:本文建立了猪肉样品中痕量氨基糖苷类抗生素(AminoglycosidesAGs)(阿米卡星、安普霉素、潮霉素B、卡那霉素、巴龙霉素、核糖霉素、大观霉素、链霉素、妥布霉素)残留的检测方法。猪肉样品经过冷冻干燥、研磨后,加入150 mmol/L EDTA溶液和5%TCA溶液进行超声提取,经Oasis HLB柱净化后,采用BEH Z-HILIC色谱柱,进行超高效液相色谱-串联质谱分析。9AGs0.01~5 μg/mL范围内线性关系良好,相关系数(R2)均大于0.999猪肉样品中AGs的定量限为0.01~0.29 μg/g。在低、中、高3种加标水平下,猪肉样品中AGs的平均加标回收率为79.91%~113.20%,相对标准偏差为1.26%~12.40%该方法操作简单、灵敏度高,适用于猪肉中AGs残留的检测

关键词:氨基糖苷类抗生素;固相萃取;超高效液相色谱-串联质谱法;猪肉

中图分类号O658              文献标A              文章编号0258-3283202501-0086-06

DOI10.13822/j.cnki.hxsj.2024.0456

 

Determination of 9 Aminoglycosides Antibiotic in Pork by Solid Phase Extraction- Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry  ZHOU Han-lin1, GUO Hang-ting1, ZHANG Hong*1, CHEN Xin-wang*2, HAN Yong-he1, ZHANG Yong1, BEN Yu-jie3 (1a.College of Environmental and Resource Science, College of Carbon Neutral Modern Industry, 1b.Fujian Normal University, Fujian Key Laboratory of Pollution Control and Resource Reuse, Fuzhou 350117, China2. Department of Pulmonary and Critical Care Medicine, Fujian Medical University Union Hospital, Fuzhou 350001, China3. Eastern Institute of Technology, Ningbo, Ningbo 315200, China.)

AbstractThe method was developed for the determination of trace aminoglycoside antibiotics (AGs) (Amikacin, Apramycin, Hygromycin B, Kanamycin, Paromomycin, Ribostamycin, Spectinomycin, Streptomycin, Tobramycin) residues in pork sample. The pork samples were freeze-dried and ground, then ultrasonically extracted by adding 150 mmol/L EDTA solution and 5% TCA solution, cleaned up by an Oasis HLB column, and then analyzed by ultra-performance liquid chromatography-tandem mass spectrometry. The linear relationships of the 9 AGs were in a good range of 0.01~5 μg/mL (R20.999). The limits of quantitation were in the range of 0.01~0.29 μg/g. At the three low, medium, and high spiking levels, the average spiking recovery rates of AGs in pork samples ranged from 79.91% to 113.20%, with relative standard deviations of 1.26% to 12.40%. This method is simple, sensitive, and suitable for detecting AGs residues in pork.

Key wordsaminoglycoside antibiotics; solid phase extraction; ultra-performance liquid chromatography-tandem mass spectrometry; pork


胶体金免疫层析法快速检测动物源食品中的诺氟沙星

 

陈文硕1温宇浩2娄婷婷3潘红蕊*1,李金花*2

(1. 天津海关工业产品安全技术中心,天津  3004572. 中国科学院烟台海岸带研究所 海岸带生态环境监测技术与装备山东省工程研究中心 山东省海岸带环境过程重点实验室,山东 烟台  2640033. 天津科技大学 生物工程学院,天津  300222)

 

摘要:胶体金免疫层析法具有高特异性、高灵敏度、高重复性等特点,能够准确地检测出样品中的目标物,在快速检测领域具有广泛应用。本研究将胶体金免疫层析法用于快速检测动物源食品(猪肉、鸡肉、鱼肉、虾肉、鸡蛋)中的诺氟沙星(Norfloxacin, NOR)残留,对方法进行验证,相对准确度为97.0%。方法的检出限2 μg/kg检测性能强。在上述5种不同基质样品中,NOR胶体金快速检测方法的灵敏度为99%、特异度为98%、假阳性率为2%、假阴性率为1%。该方法简单快速、灵敏准确,适于复杂基质中NOR的快速精准检测 

关键词:胶体金免疫层析法;诺氟沙星;方法验证;动物源食品;快速检测

中图分类号O657.31            文献标A            文章编号0258-3283202501-0092-05

DOI10.13822/j.cnki.hxsj.2024.0329

 

Rapid Detection of Norfloxacin in Animal-Derived Foods by Colloidal Gold Immunochromatography  CHEN Wen-shuo1, WEN Yu-hao3, LOU Ting-ting2, PAN Hong-rui*1, LI Jin-hua*3 (1. Industrial Product Safety Technology Center, Tianjin Customs, Tianjin 300457, China; 2. Shandong Key Laboratory of Coastal Environmental Processes, Coastal Zone Ecological Environment Monitoring Technology and Equipment Shandong Engineering Research Center, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China; 3. School of Bioengineering, Tianjin University of Science and Technology,Tianjin 300222, China) 

AbstractColloidal gold immunochromatography has the characteristics of high specificity, high sensitivity, and high repeatability, which can accurately detect the targeted analytes in the samples, and has a wide range of applications in the field of rapid detection. This study used colloidal gold immunochromatography to rapidly detect norfloxacin (NOR) residues in animal-derived foods (pork, chicken, fish, shrimp, and eggs) and validated the method with a relative accuracy of 97.0%. The limit of detection was down to 2 μg/kg, showing high detectability. By testing the above-mentioned five different matrix samples, the NOR colloidal gold rapid detection method attained a sensitivity of 99%, specificity of 98%, false positive rate of 2%, and false negative rate of 1%. This method proved simple, rapid, sensitive, and accurate, and thereby was practically applicable for the rapid, precise detection of NOR in complicated matrices.

Key wordscolloidal gold immunochromatography; norfloxacin; method validation; animal-derived foods; rapid detection


基于P&T-GC-MS技术的甲醇试剂中苯系物本底研究

 

王巧云*1,张海宇1王海燕1马名扬2

1. 广东轻工职业技术大学,广东 广州  5103002. 中国广州分析测试中心 广东省化学危害应急检测技术重点实验室,广东 广州  510070

 

摘要:苯系物是衡量水质的重要指标之一,是水环境监测优先管控的主要污染物。生活饮用水,尤其水源地水中通常并不希望检出苯系物,这些水体中苯系物的含量一般不高,浓度在方法检出限附近因此分析过程所用试剂,尤其是标样配制必不可少的甲醇中是否存在苯系物杂质,存在情况如何,对水中低浓度苯系物的准确测定非常关键。吹扫捕集-气相色谱-质谱联用法(P&T-GC-MS)具有较好的分离度和灵敏度,且进样量少、干扰小,是水中痕量苯系物检测的优选方法。本研究基于P&T-GC-MS法,开展甲醇试剂的苯系物本底研究,探索实验室常用甲醇试剂中的苯系物杂质对定量结果的影响程度和影响规律,为环境监测相关工作和研究提供数据支持。

关键词:甲醇试剂;苯系物;本底研究;吹扫捕集-气相色谱-质谱联用法(P&T-GC-MS);痕量分析

中图分类号:O657.63        文献标识码:A              文章编号:0258-3283202501-0097-08

DOI10.13822/j.cnki.hxsj.2024.0385

 

Background Study on Benzene Analogies in Methanol Reagent by Purge and Trap-Gas Chromatography-Mass Spectrometry WANG Qiao-yun*1, ZHANG Hai-yu1, WANG Hai-yan1MA Ming-yang2 (1. Guangdong Industry Polytechnic University, Guangzhou 510300, Guangdong, China; 2. Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals, China National Analytical Center, Guangzhou 510070, Guangdong, China)

Abstract: Benzene analogies are main indicators for assessing water quality and are prioritized pollutants for water environmental monitoring and control. The occurrence of benzene analogies in drinking water, particularly in source water, is generally considered to be undesirable. The concentrations of benzene analogies in such water bodies are typically low, with test results close to the detection limits of analytical methods. Therefore, the meticulous consideration of benzene analogies as impurities in the reagents utilized during sample analysis is imperative for the precise detection of these compounds at minimal concentrations in authentic samples. As an essential reagent for preparing standard samples of benzene analogies, methanol should be given special attention. The Purge and Trap-Gas Chromatography-Mass Spectrometry (P&T-GC-MS), with its good separation, high sensitivity, low sample injection volume, and minimal interference, is an optimal method for detecting trace amounts of benzene analogies in water. Based on the P&T-GC-MS method, this study investigated the background levels of benzene analogies in several commonly used methanol reagents in laboratories, explored the influence of benzene analogies on quantitative results, and provided data support for related environmental monitoring research.

Key words: methanol reagent; benzene analogies; background study; Purge and Trap-Gas Chromatography-Mass Spectrometry (P&T-GC-MS); trace analysis

 

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