【综述与专论】
高纯溶剂应用及行业高质量发展展望
全灿
(中国计量科学研究院，北京 100029）
摘要：化学工业是国民经济的基干产业，在区域经济的许多部门发挥着至关重要的作用。高纯溶剂作为基础化工材料，服务国民经济主战场，与人们生产生活密接相关。绿色溶剂助力实现人类命运共同体和联合国可持续发展目标。首先介绍高纯溶剂的国内外市场应用，国际高纯溶剂行业发展趋势、市场以及增长动能，在此基础上，应我国高质量发展需求，展望高纯溶剂如何服务我国国民经济主战场，如何服务国家重大需求，重点介绍高纯溶剂标准物质研制以建立溯源性、电子级高纯溶剂标准化满足半导体行业重大需求以及生物基溶剂满足行业绿色环保发展需求。
关键词：高纯溶剂；市场；应用；高质量发展；标准物质；电子级；生物基溶剂
中图分类号：TQ42 文献标识码：D 文章编号：0258-3283（2024）01-0001-07
DOI：10.13822/j.cnki.hxsj.2022.0838
Application of High Purity Solvents and Prospects for High Quality Development of the Solvents Industry QUAN Can (National Institute of Metrology, Beijing 100029,China)
Abstract：The chemical industry, the basic industry of the national economy, plays a vital role in many sectors of the regional economy. As a basic chemical material, high purity solvent serves the main battlefield of national economy and is closely related to people's production & life. Green solvents help to achieve the sustainable development goals of the community with a shared future for mankind and the United Nations. This paper firstly introduces the application of high purity solvents in global markets, the development trend, the growth momentum of the international high purity solvent industry. On this basis, in response to China's high-quality development needs, it looks forward to how high purity solvents can serve the main battlefield of China's national economy, and how to serve the country's major needs. It focuses on the development of high purity solvent certitied reference materials to establish tractability.The standardization of electronic grade high purity solvents meets the major needs of the semiconductor industry, and the bio-based solvents meet the green and environmental development needs of the industry.
Keywords: high purity solvent; market; application; high quality development;certified reference materials; electronic grade; bio-based solvent
引用本文：全灿. 高纯溶剂市场应用与行业高质量发展展望[J]. 化学试剂，2024，46（1）：1-7.
方氮化硼应用于样品前处理的研究进展
王伟然，张洁茹，张婉婉，张旭，熊雪*，王春英*
（河北医科大学 药学院，河北 石家庄 050011 ）
摘要：近几年，六方氮化硼由于孔隙率高、比表面积大、机械强度高、化学稳定性好、亲水性好、生物相容性好等优点，作为前处理材料获得了广泛关注，已被用于生物化学、食品安全、环境污染等领域的样品前处理，是一种理想的吸附剂。目前已开发了多种基于六方氮化硼材料作为吸附剂的样品前处理技术，包括固相萃取、分散固相萃取、固相微萃取、磁性固相萃取、管内固相微萃取、分散固相微萃取等，可实现多氯联苯、罗丹明B、黄酮类化合物、多环芳烃等分析物的萃取富集。综述了六方氮化硼材料在样品前处理领域的应用进展，并对今后的发展方向进行了展望。
关键词：六方氮化硼；样品前处理；固相萃取；分散固相萃取；固相微萃取；磁性固相萃取
中图分类号：O65 文献标识码：A 文章编号：0258-3283（2024）01-0008-09
DOI：10.13822/j.cnki.hxsj.2023.0638
Research Progress on the Application of Hexagonal Boron Nitride in Sample Preparation WANG Wei-ran, ZHANG Jie-ru, ZHANG Wan-wan, ZHANG Xu, XIONG Xue* ,WANG Chun-ying* (School of Pharmacy, Hebei Medical University, Shijiazhuang 050011, China)
Abstract: In recent years, hexagonal boron nitride has gained widespread attention as a preparation material due to its high porosity, large specific surface area, high mechanical strength, good chemical stability, good hydrophilicity, and good biocompatibility. It has been used for sample preparation in fields such as biochemistry, food safety, and environmental pollution, and it is an ideal adsorbent. At present, a variety of sample preparation technologies based on hexagonal boron nitride materials as adsorbent have been developed, including solid phase extraction, dispersive solid phase extraction, solid phase microextraction, magnetic solid phase extraction, in tube solid phase microextraction, dispersive solid-phase microextraction, etc. Based on this, hexagonal boron nitride can realize the extraction and enrichment of analytical substances such as polychlorinated biphenyls, rhodamine B, flavonoids, polycyclic aromatic hydrocarbons, etc. This article reviews the application progress of hexagonal boron nitride materials in the field of sample preparation, and prospects the future development direction.
Key words: hexagonal boron nitride; sample preparation; solid phase extraction; dispersive solid phase extraction; solid phase microextraction; magnetic solid phase extraction
引用本文：王伟然, 张洁茹, 张婉婉, 等. 六方氮化硼应用于样品前处理的研究进展[J].化学试剂, 2024, 46(1)：8-16.
雷公藤红素的结构修饰及抗肿瘤活性研究进展
陈倩虹，周婷，李媚，彭佳，米杰，覃丽，王福东*
(湖南中医药大学 药学院，湖南 长沙 410208)
摘要：雷公藤红素是一种来源于药用植物雷公藤(Tripterygium wilfordii Hook.f.)的五环三萜类天然活性产物，具有显著而广泛的抗肿瘤活性，但由于水溶性差、毒副作用强等缺点限制了其转化为临床抗肿瘤药物。为此，通过结构修饰，改善其临床应用的局限性成为该研究领域的热点。迄今，针对其进行的结构修饰主要集中于A环C-2、C-3位，B环的C-6位及E环的28位，主要有酯化、酰胺化及引入药效基团等修饰，此外，部分非常见的修饰位点同样对抗肿瘤活性有重要影响。综述了近年来雷公藤红素的结构修饰及其抗肿瘤活性研究进展，为深入研究雷公藤红素的临床应用提供参考。
关键词：雷公藤红素；结构修饰；衍生物；抗肿瘤活性；构效关系
中图分类号：R914.4 文献标识码：A 文章编号：0258-3283（2024）01-0017-09
DOI：10.13822/j.cnki.hxsj.2023.0616
Research Advances in Structural Modification and Antitumor Activity of Celastrol CHEN Qian-hong, ZHOU Ting, LI Mei, PENG Jia, MI Jie, QIN Li, WANG Fu-dong* (School of Pharmacy, Hunan University of Chinese Medicine, Changsha 410208, China)
Abstract: Celastrol, a kind of natural active product of pentacyclic triterpenes, roots in medicinal plant Tripterygium wilfordii Hook. f. It possesses significant and extensive antitumor activity. However, due to poor water solubility, strong toxic side effects and other disadvantages, its conversion into clinical antitumor drugs is limited. Therefore, improving its limitations of clinical applications through structural modification has attracted much attention in the research field. To date, the modification sites of celastrol mainly focused on the C-2, C-3 position of the ring-A, the C-6 position of ring-B, and the 28 position of the ring-E, including esterification, amidation, and introduction of pharmacological groups. In addition, some uncommon modification sites also have a significant impact on antitumor activity. The research progress of structural modification and antitumor activity of celatrol in recent years are reviewed, providing reference for intensive study on clinical application of it.
Key words: celastrol; structural modification; derivatives; anti-tumor activity; structure-activity relationship
引用本文：陈倩虹，周婷，李媚，等. 雷公藤红素的结构修饰及抗肿瘤活性研究进展[J]. 化学试剂，2024，46（1）：17-25.
【生化与药用试剂】
紫檀芪查尔酮衍生物的合成及抗肿瘤活性研究
陈诚1，李光耀1，常皓云1，王若玲1，文峻1，黄鹏*1,2，胡海霞*1,2
（1. 安徽中医药大学 药学院，安徽 合肥 230012；
2. 中药研究与开发安徽省重点实验室，安徽 合肥 230012）
摘要：以紫檀芪为先导化合物，将其酚羟基甲氧基化，引入醛基，并与丹皮酚乙酸通过羟醛缩合反应合成紫檀芪查尔酮苯氧乙酸，再与不同的有机胺反应得到10个目标化合物。所有目标化合物经核磁共振氢谱、质谱进行结构确证。采用MTT法初步评价目标化合物对人肝癌细胞HepG2、人非小细胞肺癌细胞A549、人骨肉瘤细胞U-2OS的体外抗肿瘤活性，同时采用ELISA法检测目标化合物对组蛋白去乙酰化酶（HDAC）的抑制能力。结果表明大部分目标化合物抗肿瘤活性高于紫檀芪，其中化合物5a对U-2OS细胞的IC50值达到了（6.10±1.11） μmol/L。同时，该化合物在25 μmol/L时，对HDAC1和HDAC2的抑制率可达40%左右。
关键词：紫檀芪；查尔酮；合成；抗肿瘤活性; 组蛋白去乙酰化酶
中图分类号：R914 文献标识码：A 文章编号：0258-3283（2024）01-0026-08
DOI：10.13822/j.cnki.hxsj.2023.0548
Synthesis and Antitumor Activity of Pterostilbene Chalcone Derivatives CHEN Cheng 1, LI Guang-yao 1, CHANG Hao-yun1,WANG Ruo-ling1，WEN Jun1，HUANG Peng*1,2 , HU Hai-xia*1,2 (1.School of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China; 2.Anhui Province Key Laboratory of Research & Development of Chinese Medicine, Hefei 230012, China)
Abstract: Using pterostilbene as the lead compound, its phenolic hydroxyl group was methoxylated, and the aldehyde group was introduced to synthesise zitanica astragali chalcone phenoxyacetic acid via hydroxyaldehyde condensation with salvianolic acid, and synthesize 10 target compounds by reacting with different organic amines. The target compounds were confirmed by NMR hydrogen spectroscopy and mass spectrometry. MTT method was used to initially evaluate the in vitro antitumour activities of the target compounds against human hepatocellular carcinoma cells HepG2, human non-small cell lung cancer cells A549, and human osteosarcoma cells U-2OS, while the inhibitory ability of the target products against histone deacetylase (HDAC) was monitored by ELISA. The results showed that most of the target compounds had higher antitumour activities than pterostilbene, and the compound 5a reached an IC50 value of (6.10±1.11) μmol/L against U-2OS cells. Meanwhile, the compound inhibited HDAC1 and HDAC2 up to about 40% at 25 μmol/L.
Key words: pterostilbene; chalcone; synthesis; antitumour activity; HDAC
引用本文：陈诚，李光耀，常皓云，等. 紫檀芪查尔酮衍生物的合成及抗肿瘤活性研究[J]. 化学试剂，2024，46（1）：26-33.
人参多糖分散片制备工艺及其免疫活性研究
周铄1，任京1，姜子烨1，焦丽丽1，吴巍1，李慧1，张晓瑜*1
（长春中医药大学，吉林省人参科学研究院，吉林 长春，130117）
摘要：本试验旨在确定人参多糖分散片的处方、制备工艺并检测免疫活性。采用单因素实验法对崩解剂、填充剂和润滑剂进行考察，以性状、崩解时限、硬度为考察指标，优化人参多糖分散片的处方；通过对小鼠脏器指数、迟发性变态反应、吞噬指数和自然杀伤细胞活性的测定考察人参多糖分散片的免疫活性。结果表明，人参多糖分散片的优选处方为31.25%人参粗多糖作主药，38.67%微晶纤维素与19.08% α-乳糖作复合填充剂，10%交联聚乙烯吡咯烷酮作崩解剂，1%硬脂酸镁作润滑剂，50%乙醇作润湿剂。免疫活性试验结果表明，人参多糖分散片可以显著提高小鼠的脏器指数、足跖肿胀程度、吞噬指数和自然杀伤细胞活性，具有良好的免疫增强活性。其中2.50 g/(kg·bw)人参多糖分散片的免疫活性最强，可作为潜在的保健食品或营养补充剂。
关键词：人参；多糖；分散片；制备工艺；免疫活性
中图分类号：TQ461 文献标识码：A 文章编号：0258-3283（2024）01-0034-05
DOI：10.13822/j.cnki.hxsj.2023.0585
Study on Preparation Processes and Immune Activity of Ginseng Polysaccharide Dispersible Tablets Zhou Shuo1, Ren Jing1, Jiang Ziye1, Jiao Lili1, Wu Wei1, Li Hui1, Zhang Xiaoyu*1 (Jilin Ginseng Academy, Changchun University of Chinese Medicine, Changchun, 130117)
Abstract: The prescription, preparation technology and immune activity of ginseng polysaccharide dispersible tablets were determined in the study. The disintegrants, fillers and lubricants were examined using single factor experiment method. The traits, disintegration time and hardness were used to optimize the prescription of ginseng polysaccharide dispersible tablets. The organ index, delayed hypersensitivity, phagocytic index and natural killer cell activity in mice were determined to examine the immunological activity of ginseng polysaccharide dispersible tablets. The results showed that the optimum prescription of ginseng polysaccharide dispersible tablets was 31.25% ginseng crude polysaccharide as main ingredient, 38.67% microcrystalline cellulose and 19.08% α -lactose as composite filler, 10% cross-linked polyvinylpyrrolidone as disintegrant, 1% magnesium stearate as lubricant and 50% ethanol as wetting agent. The results of immunoactivity test showed that ginseng polysaccharide dispersible tablets could significantly increase organ index, foot-plantar swelling degree, phagocytic index and natural killer cell activity in mice, exhibiting good immune enhancement function. Among them, 2.50 g/kg.bw ginseng polysaccharide dispersible tablets showed the strongest immunological activity and can be used as potential health food or nutritional supplements.
Keywords: ginseng; polysaccharide; dispersible tablets; preparation processes; immunological activity
引用本文：周铄，任京，姜子烨，等. 人参多糖分散片制备工艺及其免疫活性研究[J]. 化学试剂，2024，46（1）：34-38.
白藜芦醇对小鼠3T3-F442A脂肪细胞增殖与脂肪生成的影响
刘爱萍，李佟，程亚青，张仁文，葛雅琨，张元新*
(吉林化工学院 生物与食品工程学院，吉林 吉林 132022)
摘要：研究白藜芦醇( Resveratrol，Res) 对小鼠3T3-F442A细胞增殖与脂肪生成的影响。采用MTT法检测不同剂量的Res在24、48、72 h对3T3-F442A前细胞增殖的影响，得到72 h的半抑制浓度并确定给药浓度；使用添加40 μmol/L Res的诱导分化培养基诱导3T3-F442A前脂肪细胞分化为成熟脂肪细胞，通过油红O染色法观察Res对3T3-F442A脂肪细胞脂肪生成的影响；采用实时荧光定量PCR技术、蛋白免疫印迹实验、酶联免疫吸附实验检测Res对3T3-F442A脂肪细胞分化相关转录因子（C/EBPα、C/EBPβ、PPARγ和aP2）、脂肪生成相关血管内皮生长因子及受体（VEGF-α和VEGFR-2）以及基质金属蛋白酶（MMP-2和MMP-9）表达的影响。Res以时间-剂量依赖方式抑制 3T3-F442A 前脂肪细胞增殖；Res组的脂肪细胞分化相关转录因子、血管重塑因子以及基质金属蛋白酶（MMP-2和MMP-9）mRNA表达水平均明显下调；脂肪细胞分化相关转录因子的蛋白表达水平均明显下调以及分泌到胞外的基质金属蛋白酶（MMP-2和MMP-9）的浓度也明显下降。Res能抑制 3T3-F442A 前脂肪细胞增殖与脂肪生成，其机制可能是通过抑制与基质金属蛋白酶（MMP-2和MMP-9）相关的血管生成过程而发生的。
关键词：脂肪细胞；白藜芦醇；转录因子；基质金属蛋白酶；分化
中图分类号：R285.5 文献标识码：A 文章编号：0258-3283（2024）01-0039-06
DOI：10.13822/j.cnki.hxsj.2023.0511
Effects of Resveratrol on Cell Proliferation and Adipogenesis in Murine 3T3-F442A Preadipocytes LIU Ai-ping, LI Tong, CHENG Ya-qing, ZHANG Ren-wen, GE Ya-kun, ZHANG Yuan-xin* ( College of Biology and Food Engineering, Jilin Institute of chemical technology, Jilin 132022, China)
Abstract：The effects of Resveratrol (Res) on the Proliferation and adipogenesis of 3T3-F442A cells in mice were investigated. The effects of different doses of Res on the Proliferation of 3T3-F442A Preadipocytes at 24, 48 and 72 h were detected by MTT assay, and the semi-inhibitory concentration at 72 h was obtained and determined the optimal concentration; and then 3T3-F442A Preadipocytes were induced to differentiate into mature adipocytes by using the induced differentiation medium with the addition of 40 μmol/L Res, and the effects of Res on the adipogenesis of 3T3-F442A adipocytes were observed by the oil-red O staining method. Quantitative Real-time PCR, Western blot, and enzyme-linked immunosorbent assay were used to detect the effects of Res on 3T3-F442A adipocyte differentiation-associated transcription factors (C/EBPα, C/EBPβ, PPARγ, and aP2), adipogenesis-associated vascular endothelial growth factor and receptors (VEGF-α and VEGFR-2), and matrix metalloproteinases (MMP-2 and MMP-9) expression. Res inhibited the Proliferation of 3T3-F442A Preadipocytes in a time-dose-dependent manner; mRNA expression levels of adipocyte differentiation-associated transcription factors, vascular remodelling factors, and matrix metalloproteinases (MMP-2 and MMP-9) were significantly down-regulated in the Res group, and Protein expression levels of adipocyte differentiation-associated transcription factors were significantly down-regulated, as well as the levels of matrix metalloproteinases (MMP-2 and MMP-9) secreted into the extracellular compartment. Res inhibited the Proliferation and adipogenesis of 3T3-F442A preadipocytes, probably by inhibiting the angiogenic process associated with matrix metalloproteinases (MMP-2 and MMP-9).
Key words：adipocyte; resveratrol; transcription factor; matrix metalloproteinase; differentiation
引用本文：刘爱萍，李佟，程亚青，等. 白藜芦醇对3T3-F442A脂肪细胞的增殖与脂肪生成的影响[J]. 化学试剂，2024，46（1）：39-44.
【功能材料】
基于螺噁嗪光异构化的多功能荧光染料及应用
刘箫音，杨素华*，张寒，魏云杰，王会东，辛景凡，曹瑞
(赤峰学院 化学与生命科学学院 内蒙古自治区光电功能重点实验室，内蒙古 赤峰 024000)
摘要：合成了键合萘酰亚胺单元的螺噁嗪类化合物Ⅴ，通过核磁共振谱和高分辨质谱确证了其结构。紫外光照射后，化合物能发生从浅黄色到绿色开环体的异构化反应，同时萘酰亚胺单元的荧光强度有所降低。化合物在H+存在时经紫外光照射后发生从浅黄色变为橙色或红色的颜色改变（生成MCH+），其最大吸收波长与萘酰亚胺单元的荧光发射波长具有很好的交叠，发生明显的荧光共振能量转移(FRET)，可见光能使逆过程发生伴随着颜色和荧光的恢复，这些结果赋予化合物紫外光/可见光交互作用下的可逆荧光分子开关功能。化合物在滤纸上氢离子存在或缺失条件下的颜色及荧光改变的区别，显示了化合物在多重防伪领域中的应用潜力。
关键词：螺噁嗪；光致变色；萘酰亚胺；酸致变色；荧光共振能量转移
中图分类号：O657.3 文章标识码：A 文章编号：0258-3283（2024）01-0045-08
DOI：10.13822/j.cnki.hxsj.2023.0647
Multifunctional Fluorescent Dyes based on Spirooxazine Photoisomerization and Its Applications LIU Xiao-yin, YANG Su-hua*, ZHANG Han， WEI Yun-jie , WANG Hui-dong, XIN Jing-fan, CAO Rui (Inner Mongolia Key Laboratory of Photoelectric Functional Materials, College of Chemistry and Life Sciences, Chifeng university, Chifeng 024000, China)
Abstract: A novel spiroxazine compound Ⅴ with naphthalimide unit was synthesized and its structure was confirmed by NMR and HRMS. The solution color of Ⅴ changes from light yellow (SO form) to green (MC form) once they are subjected to ultraviolet (UV) irradiation, accompanied by a certain decrease in the fluorescence intensity of the naphthalimide unit. The compound undergoes a color change from light yellow to orange or red (another type of open ring form MCH+) upon UV irradiation in the presence of H+. The maximum absorption wavelength of MCH can overlap with the emission wavelength of the naphthalimide unit at 500-550 nm. Thus, fluorescence resonance energy transition (FRET) may happen between the MCH and 1,8-naphthalimide units, while the reverse isomerization will be conducted with visible light accompanied by recovery of color and fluorescence. The results indicates that the compound exhibits excellent fluorescence molecular switching function under the interaction of UV and Vis. The color and fluorescence changes of the compound in the presence or absence of hydrogen ions in filter paper were tested, demonstrating its potential application in multiple anti-counterfeiting fields.
Key words: spirooxazine; photochromism; naphthalimide; acidichromism; FRET
引用本文：刘箫音，杨素华，张寒，等. 基于螺噁嗪光异构化的多功能荧光染料及应用[J]. 化学试剂，2024，46（1）：45-52.
【电化学和新能源】
二硒化钴电催化剂的制备及氧还原性能测试
杨晓玲*a，孙怡然a，晁佳钰a，支东彦a，陈健壮a，沈建华b
(华东理工大学 a. 材料国家级实验教学示范中心，b. 材料科学与工程学院，上海 200237)
摘要：具有高附加值的绿色环保型氧化剂—过氧化氢（H2O2）的需求日益增加，急需发展绿色且安全的H2O2合成新方法。两电子氧还原反应（2e-ORR）是一种制备H2O2的高效方法，其中催化剂的高效率和高选择性是2e-ORR的关键。对二硒化钴（CoSe2）电催化剂的制备和性能测试实验进行了探索。首先，通过联氨还原法制备钴纳米粒子；然后，通过简单的固相反应并在不同温度下退火制备CoSe2电催化剂；最后，通过一系列的表征方法对CoSe2电催化剂的表面形貌、晶型、电化学及其稳定性等进行了研究。为2e-ORR电催化剂CoSe2的进一步研究和应用开发提供借鉴。
关键词：氧还原反应；过氧化氢；固相反应；CoSe2；电催化剂
中图分类号：G642.0 文献标识码：A 文章编号：0258-3283（2024）01-0053-06
DOI：10.13822/j.cnki.hxsj.2023.0554
Preparation and Oxygen Reduction Performance Test of Cobalt Diselenide Electrocatalytic YANG Xiao-ling*a, SUN Yi-rana, CHAO Jia-yua, ZHI Dong-yana, CHEN Jian-zhuanga, SHEN Jian-huab (a. National Demonstration Center for Experimental Material Education, b. School of Materials Science and Engineering, East China University of Science and Technology, Shanghai 200237, China)
Abstract：With the increasing demand of highly value-added and environment-friendly oxidant hydrogen peroxide (H2O2), it is urgent to develop a new green and safe synthesis method of H2O2. Two-electron oxygen reduction reaction is an efficient method to prepare H2O2, in which the high efficiency and selectivity of catalyst is the key factors for 2e-ORR. The preparation and performance test of cobalt diselenide(CoSe2) electrocatalyst were investigated in this paper. Firstly, cobalt nanoparticles were prepared by hydrazine reduction method. Then, CoSe2 electrocatalyst was prepared by simple solid phase reaction and annealing at different temperatures. Finally, the surface morphology, crystal phase, electrochemistry and stability of CoSe2 electrocatalyst were studied by a series of characterization methods. This work will benefit the further research and application of 2e-ORR electrocatalyst CoSe2.
Key words：oxygen reduction reaction; hydrogen peroxide; solid phase reaction; CoSe2; electrocatalyst
引用本文：杨晓玲，孙怡然，晁佳钰，等.二硒化钴电催化剂的制备及氧还原性能测试[J]. 化学试剂，2024，46（1）：53-58.
【化学品与环境】
3种方法制备NiCoCr-LDHs对MO的吸附性能研究
蒋以晨，田慧媛，夏梦岩，李阳，崔节虎*
（郑州航空工业管理学院 材料学院，河南 郑州 450000)
摘 要：本文使用尿素水解法（Urea）、恒定pH共沉淀法（CC-H）、超声共沉淀法（U-H）制备了新型NiCoCr-LDHs吸附剂，研究其在各种因素条件下对甲基橙染料废水的吸附性能的影响，并对3种NiCoCr-LDHs吸附实验的结果进行分析与评价。结果表明：不同方法制备3种NiCoCr-LDHs吸附行为均符合Langmuir等温吸附和准二级动力学模型，表明3种材料是以单层吸附和层间离子交换为主。Urea、CC-H、U-H制备材料的最大吸附容量分别为355、390和278 mg/g，不同制备技术使3种吸附剂在表面结构、比表面积等方面有较大区别，最终导致在吸附过程中最大吸附量有显著差别，并简要分析了其吸附机理。
关键词：NiCoCr-LDHs；甲基橙；吸附；单层吸附；化学吸附
中图分类号：X703 文献标识码：A 文章编号：0258-3283（2024）01-0059-10
DOI：10.13822/j.cnki.hxsj.2023.0560
Study on the Adsorption Performance of NiCoCr-LDHs Prepared by Three Methods for MO JIANG Yi-chen, TIAN Hui-yuan, XIA Meng-yan, LI yang, Cui Jie-hu (Zhengzhou University of Aeronautics,School of Materials, Zhengzhou, Henan 450000)
Abstract: In this paper, a new type of NiCoCr-LDHs adsorbent was prepared by urea hydrolysis method (Urea), constant pH coprecipitation method (CC-H) and ultrasonic coprecipitation method (U-H). The adsorption performance of NiCoCr-LDHs on methyl orange dye wastewater under different factors was investigated, and its adsorption behavior was evaluated. The research results indicate that: The adsorption behavior of three NiCoCr-LDHs preparation using different methods conforms to Langmuir adsorption isotherm model and quasi second-order kinetic model, which indicated that the three materials are mainly monolayer adsorption and interlayer ion exchange. The maximum adsorption capacities of Urea, CC-H, and U-H prepared materials are 355, 390, and 278 mg/g, respectively. The surface structure, specific surface area, and other aspects of the three adsorbents vary greatly due to different preparation techniques, which also leads to different adsorption capacities of the materials. This article also briefly analyzes the adsorption mechanism of NiCoCr-LDHs on MO.
Key words:NiCoCr-LDHs; MO; adsorption; monolayer adsorption; chemical adsorption
引用本文：蒋以晨，田慧媛，夏梦岩，等. 3种方法制备NiCoCr-LDHs对MO的吸附性能研究[J]. 化学试剂，2024，46（1）：59-68.
the Ti3C2Tx ultra-thin nanosheets were characterized by SEM, XRD, FT-IR and Raman. The contents of heavy metal ions in the waste water before and after treated by Ti3C2Tx nanosheets were determined by ICP-MS. A large number of functional hydroxyl groups and structure defects were found on the nanosheet surface. When the initial concentration of Cu (II), Pb (II), and Cr (VI) ions in the water was 50 mg/L, the removal efficiency of 47.5 mg Ti3C2Tx nanosheets to the metal ions was over 90%, especially for Pb (II) ions, which reached as high as 98.81%. The adsorption performance is much higher than the adsorption reagents such as macroporous resin, acid washed diatomaceous earth, and activated carbon. In the coexisting solutions of Na (I), Cu (II), Pb (II), and Cr (VI) ions, the removal of Pb (II) and Cr (VI) by Ti3C2Tx nanosheets can still reach over 92%. And the adsorption of Pb (II) by Ti3C2Tx nanosheets was conformed in agreement with the pseudo second-order kinetic model and Langmuir isotherm model, and the maximum adsorption capacity and detection limit for Pb (II) are ca. 81.7 mg/g and 0.0094 mg/L, respectively. Adsorption of heavy metal ions by Ti3C2Tx ultra-thin nanosheets has a good application prospect in wastewater treatment for the chemical industry and food processing fields.
Key words: Ti3C2Tx; ultra-thin nanosheets; heavy metal ions; etching and stripping; adsorption
引用本文：蒋以晨，田慧媛，夏梦岩，等. 3种方法制备NiCoCr-LDHs对MO的吸附性能研究[J]. 化学试剂，2024，46（1）：59-68.
Ti3C2Tx超薄纳米片高效率去除废水中重金属的研究
于雪荣*，姜健，王秀莉，陈元元，刘惠，陈宁宁
（安徽省疾病预防控制中心 理化检验室，安徽 合肥 230601）
摘要：通过刻蚀剥离法制备了Ti3C2Tx超薄纳米片，探究了其对废水中重金属离子的吸附特性。通过SEM、XRD、AFM、FT-IR、Raman对Ti3C2Tx超薄纳米片的形貌和结构进行了表征，通过ICP-MS对处理前后水体中重金属离子的含量进行了测试。结果表明剥离的Ti3C2Tx超薄纳米片表面含有结构缺陷和羟基，当水体中Cu (II)、Pb (II)、Cr(VI)初始浓度为50 mg/L时，47.5 mg Ti3C2Tx超薄纳米片对其的去除效率高达90%以上，尤其是对Pb (II)的去除效率达到了98.81%，吸附性能远高于大孔树脂、硅藻土和活性炭等常见吸附试剂。在Na(I)、Cu(II)、Pb (II)、Cr (VI)4种离子共存溶液中，Ti3C2Tx超薄纳米片对于Pb (II)和Cr (VI)的去除依然可以达到92%以上。通过动力学和吸附等温拟合，Ti3C2Tx纳米片对Pb (II)的吸附符合拟二级动力学模型和Langmuir等温模型，对Pb (II)的最大吸附量和最低检出限分别为81.7 mg/g和0.0094 mg/L。Ti3C2Tx超薄纳米片对重金属离子的吸附特性在化学工业、食品加工的废水处理中具有良好的应用前景。
关键词：Ti3C2Tx；超薄纳米片；重金属；刻蚀剥离；吸附
中图分类号：TE991.2 文献标志码：A 文章编号：0258-3283（2024）01-0069-07
DOI：10.13822/j.cnki.hxsj.2023.0590
High Efficiency Removal of Heavy Metal Ionsfrom Wastewater using Ti3C2Tx Ultra-thin Nanosheets YU Xue-rong*, JIANG Jian, WANG Xiu-li，CHEN Yuan-yuan，LIU Hui, CHEN Ning-ning (Physics and Chemistry Lab, Anhui Center for Disease Control and Prevention, Hefei 230601, China)
Abstract: Ultra-thin Ti3C2Tx nanosheets were prepared by etching and stripping, and their adsorption properties to heavy metal ions were studied. The morphology and structure of the Ti3C2Tx ultra-thin nanosheets were characterized by SEM, XRD, FT-IR and Raman. The contents of heavy metal ions in the waste water before and after treated by Ti3C2Tx nanosheets were determined by ICP-MS. A large number of functional hydroxyl groups and structure defects were found on the nanosheet surface. When the initial concentration of Cu (II), Pb (II), and Cr (VI) ions in the water was 50 mg/L, the removal efficiency of 47.5 mg Ti3C2Tx nanosheets to the metal ions was over 90%, especially for Pb (II) ions, which reached as high as 98.81%. The adsorption performance is much higher than the adsorption reagents such as macroporous resin, acid washed diatomaceous earth, and activated carbon. In the coexisting solutions of Na (I), Cu (II), Pb (II), and Cr (VI) ions, the removal of Pb (II) and Cr (VI) by Ti3C2Tx nanosheets can still reach over 92%. And the adsorption of Pb (II) by Ti3C2Tx nanosheets was conformed in agreement with the pseudo second-order kinetic model and Langmuir isotherm model, and the maximum adsorption capacity and detection limit for Pb (II) are ca. 81.7 mg/g and 0.0094 mg/L, respectively. Adsorption of heavy metal ions by Ti3C2Tx ultra-thin nanosheets has a good application prospect in wastewater treatment for the chemical industry and food processing fields.
Key words: Ti3C2Tx; ultra-thin nanosheets; heavy metal ions; etching and stripping; adsorption
引用本文：于雪荣，姜健，王秀莉，等. Ti3C2Tx超薄纳米片高效率去除废水中重金属的研究[J].化学试剂，2024，46（1）：69-75.
【分析与测试】
不同贮存年份的大别山区野生花椒精油成分分析及
抗氧化活性测定
叶兆伟1,2，陈卫1，马晓辉2，乔林1，王海燕1,2，郭磊磊1，陈琼*1,2
（1. 信阳农林学院 制药工程学院，河南 信阳 464000；2. 河南省大别山林药生态种植工程技术研究中心，河南 信阳 464000）
摘要：为了分析不同贮存年份的大别山区野生花椒精油成分，并测定不同贮存年份花椒所提取精油的抗氧化能力，采用HS-GC-MS（顶空气相色谱-质谱联用）技术对其挥发性成分进行分析；采用DPPH法测定花椒精油的抗氧化活性。结果表明，当年采收的花椒其精油提取率为2.3±0.17（mL/100g），贮存1年和贮存2年的花椒其精油提取率分别为2.0±0.14、1.8±0.25（mL/100g）。当年采收的花椒其精油中分离有效成分23种，主要有1-甲基-4-（1-甲基乙烯基）环己烯（34.44%）、桉叶油醇（8.27%）、(Z)-9-十八烷酸甲酯（8.14%）、1-甲基-4-(1-甲乙基)-1,3-环己二烯（7.87%）、1-甲基-4-(1-甲基乙基)-1,4-环己二烯（7.67%）；贮存1年的花椒其精油中分离有效成分15种，主要有(S)-(-)-柠檬烯（32.95%）、β-月桂烯（14.65%）、桉叶油醇（11.9%）、γ-松油烯（7.43%）、α-松油烯（7.27%）；贮存2年的花椒其精油中分离有效成分为12种，主要有1-甲基-4-(1-甲基乙烯基)-环己醇乙酸酯（27.01%）、β-月桂烯（23.36%）、萜烯（21.67%）、桉叶油醇（10.45%）、α-蒎烯（9.12%）。花椒精油浓度为16%时对DPPH的清除率最高，当年、贮存1年和贮存2年的花椒其精油清除率分别达77.3%、64.7%、52.5%。因此，不同贮存年份的大别山区野生花椒其精油提取率随着贮存年份的延长而降低；精油的化学成分及其含量也有不同程度的改变；不同贮存年份的大别山区野生花椒其精油均具有抗氧化能力，抗氧化能力亦随着贮存年份的延长而降低，因此，在食品、保健品和香料香精等行业中使用花椒精油时，尽量使用当年采收的花椒。
关键词：贮存年份；大别山区；野生花椒；精油；HS-GC-MS；抗氧化；DPPH法
中图分类号：TQ 文献标识码：A 文章编号：0258-3283（2024）01-0076-07
DOI：10.13822/j.cnki.hxsj.2023.0598
Different Storage Time on Composition Analysis and Antioxidant Activity of Essential Oils from Wild Zanthoxylum bungeanum in Dabie mountain area YE Zhao-wei1,2, CHEN Wei1, MA Xiao-hui2, QIAO Lin1, WANG Hai-yan1,2, GUO Lei-lei1, CHEN Qiong*1,2 (1. School of biology and pharmaceutical engineering , Xinyang Agriculture and Forestry University , Xinyang 464000, Henan China；2. Dabie Mountain Forest-medicine Ecological Planting Engineering and Technology Research Center of Henan Province, Xinyang 464000, Henan China)
Abstract: To analyze the composition and determine antioxidant activity of essential oils from wild zanthoxylum bungeanum in Dabie mountain area with different storage years, HS-GC-MS (Headspace Gas Chromatography-Mass Spectrometry ) technology was selected to analyze the essential oils, components. The antioxidative activity was investigated with the ability of scavenging DPPH as an index. The results show that the extraction rate of essential oils from wild zanthoxylum bungeanum in Dabie mountain area is 2.3±0.17 (mL/100g), 2.0±0.14 (mL/100g), 1.8±0.25 (mL/100g) stored for current year, 1 year and 2 year respectively. Twenty-three active components were isolated from the essential oils of peppercorns harvested in the same year. Fifteen and twelve active components were isolated from the essential oils of peppercorns stored for 1 year and 2 year respectively. The main components of essential oil from wild zanthoxylum bungeanum stored for current year include (S)-1-methyl-4-(1-methylethenyl)- Cyclohexene (34.44%), Eucalyptol (8.27%), (Z)-9-Octadecenoic acid methyl ester (8.14%), 1-methyl-4-(1-methylethyl)-1,3-Cyclohexadiene (7.87%), Terpinene (7.67%); stored for 1 year include (S)-(−)-Limonene (32.95%), β-Myrcene (14.65%), Eucalyptol (11.9%), γ-Terpinene (7.43%), α-Terpinene (7.27%); stored for 2 year include 1-methyl-4-(1-methylethenyl)-Cyclohexanol (27.01%), β-Myrcene (23.36%), 4-methylene-1-(1-methylethyl)-Bicyclo [3.1.0] hexane (21.67%), Eucalyptol (10.45%), α-Pinene (9.12%). The highest DPPH removal rate was achieved at a concentration of 16%, with a maximum removal rate of 77.3%, 64.7%, 52.5% respectively. So the extraction rate of essential oil of wild zanthoxylum bungeanum in Dabie mountain area decreased with the extension of storage years; the chemical composition and content of essential oils also have changes and antioxidant capacity also decreased with the extension of storage years. Therefore, when using peppercorn essential oils in the food, health food and flavor and fragrance industries, try to use peppercorns harvested in the current year. Wild Zanthoxylum bungeanum in Dabie mountain area has certain development and utilization value.
Key words: storage year; Dabie mountain; wild Zanthoxylum bungeanum; essential oil; HS-GC-MS; antioxidant; DPPH method
引用本文：叶兆伟，陈卫，马晓辉，等. 不同贮存年份的大别山区野生花椒精油成分分析及抗氧化活性测定[J]. 化学试剂，2024, 46（1）：76-82.
快速过滤净化-UPLC-MS/MS同时测定畜禽肉中12种兽药残留
李楚瑶*，唐俊，万亮，郭雪梅，陈春艳，王姝
（南昌市检验检测中心 南昌市保健食品及其接触材料质量安全风险评估重点实验室，江西 南昌 330096）
摘要：采用功能化聚苯乙烯/苯聚合物为填料的快速过滤净化柱萃取畜禽肉中的兽药，再结合超高效液相色谱-串联质谱（UPLC-MS/MS）高通量分析，建立了一种可同时测定12种兽药残留的方法。通过正交试验设计筛选前处理的最佳条件，样品经pH 4.0的EDTA-Mcllvaine缓冲液提取，按压式固相过滤柱快速净化，UPLC-MS/MS检测，外标法定量。结果表明，12种兽药在较宽的线性范围内拟合良好，相关系数均大于0.99，方法检出限0.3~3 μg/kg，定量限1.0~10 μg/kg。在3个不同添加水平下，猪肉、鸡肉、牛肉样品中的回收率分别为82.8%~110.4%、80.2%~108.4%、75.8%~107.1%，RSDs为0.51%~10.23%。该方法用于市售猪肉中的兽药检测，其中恩诺沙星、环丙沙星、金霉素、土霉素、四环素和强力霉素被检测出，与国标方法的测定结果相一致。该方法简单、快速、准确，适合多种兽药残留的同步筛查和准确定量。
关键词：超高液相色谱-串联质谱；快速过滤净化；兽药残留；畜禽肉
中国分类号：O658 文献标识码：A 文章编号：0258-3283（2024）01-0083-08
DOI：10.13822/j.cnki.hxsj.2023.0603
Simultaneous Determination of 12 Veterinary Drugs in Livestock and Poultry Meat by Rapid Filter Purification Couple with Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (UPLC-MS/MS）LI Chu-yao *, TANG Jun, WAN Liang, GUO Xue-mei, CHEN Chun-yan, WANG Shu (Nanchang Key Laboratory for Quality and Safety Risk Assessment of Health Food and its Contact Materials, Nanchang Inspection and Testing Center, Nanchang 330096, China)
Abstract: Based on a rapid filtration column with functional polystyrene/benzene polymer as filler, a method was developed for simultaneous determination of 12 kinds of veterinary drug in livestock and poultry meat, combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). An orthogonal experimental design was used to determine the optimal conditions of sample pretreatment. The target analytes were extracted from the samples by EDTA-Mcllvaine buffer solution with pH 4.0, quickly purified by pressing solid phase filter column, analyzed by UPLC-MS/MS, and quantified by external standard method. The proposed method showed a good linear relationship with correlation coefficients (R2) greater than 0.99. The limits of detection (LODs) and limits of quantitation (LOQs) of the method were ranged from 0.3 to 3 μg/kg and from 1.0 to 10 μg/kg. At three spiked levels, the recoveries of 12 kinds of veterinary drugs in pork, chicken and beef samples were 82.8%~110.4%, 80.2%~108.4%, 75.8%~107.1%, respectively, and relative standard deviations (RSDs) were between 0.51%~10.23%. The developed method was successfully applied to veterinary drugs analysis in pork samples, which were bought from local markets. Six compounds of enrofloxacin, ciprofloxacin, chlortetracycline, oxytetracycline, tetracycline and doxycycline were detected, and the detection values were consistent with National Standard method. The method was suitable for simultaneous screening and rapid quantification for veterinary drug residues with the advantages of easy accessibility, rapid detection and accuracy.
Key words: ultra performance liquid chromatography-tandem mass spectrometry; rapid filter purification; veterinary drug residues; livestock and poultry
引用本文：李楚瑶，唐俊，万亮，等. 快速过滤净化-UPLC-MS/MS同时测定畜禽肉中12种兽药残留[J]. 化学试剂，2024，46（1）：83-90.
【合成与工艺技术】
氮杂吡咯西里啶类化合物的合成及抗菌活性
吴璐璐，杨国玉，江圣飞，樊小改，徐翠莲*
（河南农业大学 理学院，河南 郑州 450002）
摘要：以乙内酰脲、醛和丙二腈为原料，锌为催化剂的条件下，一锅法得到氮杂吡咯西里啶衍生物，尝试不同取代的醛，得到17种目标化合物，产率为40% ~ 94%。结果表明，以水为溶剂，温度为80℃，锌催化剂用量为10 mol%为最优反应条件。产物结构经红外光谱（IR）、核磁共振波谱（NMR）和高分辨质谱（HRMS）确证。该方法具有反应条件温和、溶剂无毒、后处理简单、产率高、催化剂可循环使用等优点。采用菌丝生长法测试了其对禾谷镰刀菌、串珠镰刀菌、尖孢镰刀菌、烟草疫霉菌和立枯丝核菌的抗菌活性。结果表明，目标化合物对供试病原菌均有一定的抑菌活性，其中化合物4d、4f、4n和4o对禾谷镰刀菌表现出较优的活性。
关键词：水相反应；锌-脯氨酸复合物；一锅法；氮杂吡咯西里啶类化合物；抗菌活性
中图分类号：0626.32+3 文献标志码：A 文章编号：0258-3283（2024）01-0091-07
DOI：10.13822/j.cnki.hxsj.2023.0617
Synthesis and Antifungal Activity of Azapyrrolizidines WU Lu-lu, YANG Guo-yu, JIANG Sheng-fei, FAN Xiao-gai, XU Cui-lian (College of Sciences, Henan Agricultural University, Zhengzhou 450002, China)
Abstract: Using hydantoin, aldehydes and malononitrile as raw materials, pyrano [2,3-c] pyrazole derivatives was synthesized in one pot with zinc catalyst. Then, 17 pyrano [2,3-c] pyrazole derivatives were obtained by different substituted aldehydes. The yield ranged from 40% to 94%. The results showed that the optimal reaction conditions are water as solvent, temperature of 80 ℃ and 10 mol% zinc as the catalyst. The target products were confirmed by nuclear magnetic resonance spectroscopy (NMR) and high resolution mass spectrometry data (HRMS). The method has the advantages of mild reaction conditions, non-toxic solvent, the simple work up procedure, high yield and reused catalyst. The mycelial growth method was used to test the antifungal activity against Fusarium graminearum, Fusarium moniliforme, Fusarium oxysporum, Phytophthora parasitica var nicotianae and Rhizoctonia solani Kuhn. The bioactivity results showed that the target compounds had certain antifungal activities. Particularly, compound 4d, 4f, 4n, 4o displayed better activity against F. graminearum.
Key words: aqueous media; Zinc-proline complex; one-pot; azapyrrolizidine derivatives; antifungal activity
引用本文：吴璐璐，杨国玉，江圣飞，等. 氮杂吡咯西里啶类化合物的合成及抗菌活性[J]. 化学试剂，2024，46（1）：91-97.
新型氧钒配合物的合成及催化乙烯（共）聚合活性研究
刘金海a，赖新鑫a，任丽a，郝俊鹏b，李小英b，吴玥莹b，卢令攀*a
(郑州工业应用技术学院 a. 河南省水环境与健康工程技术研究中心，b. 药学与化学工程学院，河南 郑州 451100)
摘要：烯烃和功能化单体共聚合是制备功能化聚烯烃的重要途径之一。在催化烯烃和功能化单体共聚合过程中，钒系过渡金属催化剂的失活是目前最具挑战的问题。为发现热稳定性好、极性单体耐受性优良的新型钒系催化剂，设计并合成了[NOON]型多齿配体螯合的新型五价氧钒配合物2a-b，并通过1HNMR、13CNMR、51VNMR以及XRD的方法确认分子结构。乙烯均聚结果表明，2a-b均能在高温下高活性催化乙烯聚合（活性最高达40.2 kg/mmolV×h），表现出良好的热稳定性。在乙烯与5-降冰片烯-2-甲醇共聚合中，2a-b同样表现出较高活性，极性单体插入率最高可达1.66%。
关键词：多齿配体；氧钒配合物；极性单体；乙烯均聚合；共聚合
中图分类号：O62 文献标识码：A 文章编号：0258-3283（2024）01-0098-07
DOI：10.13822/j.cnki.hxsj.2023.0629
Novel Oxo-vanadium Complexes: Synthesis and Study on Catalytic Properties for Ethylene (Co)Polymerization LIU Jin-haia, LAI Xin-xina, REN Lia, HAO Jun-pengb, LI Xiao-yingb, WU Yue-yingb, LU Ling-pan*a (a. Henan Engineering Research Center of Water Environment and Health, b.School of Pharmacy and Chemical Engineering, Zhengzhou University of Industrial Technology, Zhengzhou 451100, China)
Abstract: Copolymerization of olefin and functional monomer is one of the important ways to prepare functional polyolefin. The deactivation of vanadium transition metal catalysts is the most challenging problem in the copolymerization of olefin and functional monomers. In order to find novel vanadium catalysts with good thermal stability and excellent tolerance to polar monomers, novel pentavalent oxo-vanadium complexes 2a-b bearing [NOON]-type polydentate ligand were designed and synthesized. The molecular structures were confirmed by 1HNMR, 13CNMR, 51VNMR and X-ray single crystal diffraction. The results of ethylene homopolymerization show that 2a-b exhibited high activity at high temperature (up to 40.2 kg/mmolV·h), displaying good thermal stability. In the copolymerization of ethylene with 5-norbornene-2-methanol, 2a-b also showed high activity, and the insertion rate of polar monomer was up to 1.66%.
Key words：polydentate ligand; oxo-vanadium complex; polar monomer; ethylene homopolymerization; copolymerization
引用本文：刘金海，赖新鑫，任丽，等. 新型氧钒配合物的合成及催化乙烯（共）聚合活性研究[J]. 化学试剂，2024，46（1）：98-104
达比加群酯-d3的合成
王昌1，梁林辉2，姚永秀2，梁大伟*2，董金华1
(1.沈阳药科大学 基于靶点的药物设计与研究教育部重点实验室，辽宁 沈阳 110016；2.雅安职业技术学院 药学与检验学院，四川 雅安 625100)
摘要：研究抗凝血药物达比加群酯-d3的合成工艺。以4-氯-3-硝基苯甲酸甲酯为起始原料，氘代甲胺盐酸盐为氘代试剂，经氘代甲基化、取代、还原、缩合、环合、水解和氨解反应，成功制备稳定的达比加群酯-d3，八步反应总收率为6.4%，目标化合物结构经NMR和MS确认，同位素丰度达99.7%。该合成方法原料简单易得、操作简便、重现性好，可用于达比加群酯-d3的合成。
关键词：抗凝血药物；达比加群酯-d3；合成工艺；优化；同位素标记
中图分类号：O62 文献标识码：A 文章编号：0258-3283（2024）01-0105-06
DOI：10.13822/j.cnki.hxsj.2023.0575
Synthesis of Dabigatran etexilate-d3 WANG Chang1, LIANG Lin-hui2, YAO Yong-xiu2, LIANG Da-wei*2, DONG Jin-hua1 (1.Key Laboratory of Structure-based Drug Design & Discovery of Ministry of Education, Shenyang Pharmaceutical University, Shenyang 110016, China; 2. School of Pharmacy & Medical Laboratory Science, Ya’an Polytechnic College, Ya’an, 625100, China)
Abstract：To investigate the synthesis of the anticoagulant drug dabigatran etexilate-d3. Using Methyl 4-chloro-3-nitrobenzoate as the starting materials and deuteromethylamine hydrochloride as a deuterated reagent, the stable dabigatran etexilate-d3 was synthesized via deuterated methylation, substitution, reduction, condensation, cyclization, hydrolysis and ammonolysis reaction. The total yield was 6.4%, and the structure was confirmed by NMR and MS. The isotopic enrichment of dabigatran etexilate-d3 was 99.7%. The synthetic method has several advantages, such as low cost of starting materials, facile operation process, and good reproducibility. The synthetic procedure is suitable for the laboratory production of dabigatran etexilate-d3.
Key words：anticoagulant drugs; dabigatran etexilate-d3; synthetic process; optimization; isotope labeling
引用本文：王昌，梁林辉，姚永秀，等. 达比加群酯-d3的合成[J].化学试剂，2024，46（1）：105-110.
