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《化学试剂》2022年第6期中英文摘要(附整期文章PDF文档)

【综述与专论】

丝氨酸蛋白酶有机小分子荧光探针的研究进展

尧功梅1庞承云2蒙柳卫1李清*1

(1.      广西医科大学 药学院,广西 南宁  5300212.广西医科大学附属肿瘤医院 药学部,广西 南宁  530021

 

摘要丝氨酸蛋白酶与人类生命健康息息相关。人体内丝氨酸蛋白酶水平的异常会引起疾病,危害人类生命安全。丝氨酸蛋白酶荧光探针对于检测体内和体外的丝氨酸蛋白酶数量、活性动态以及临床疾病的治疗有重要意义。因此,重点回顾了近5年来文献中报道的性能优异的常见丝氨酸蛋白酶荧光探针,以各种丝氨酸蛋白酶的显色标记为出发点,总结了目前丝氨酸蛋白酶的荧光探针的合成和性能研究,旨在为丝氨酸蛋白酶的荧光探针设计策略与检测应用提供理论参考。

关键词:丝氨酸蛋白酶;荧光探针;设计策略;发光机理;性能研究;检测应用

中图分类号R944R95            文献标识码A          文章编号0258-32832022

 

Recent Advances on the Design Strategy and Application Status of Small Organic Molecular Fluorescent Probes of Serine Protease YAO Gong-mei1, PANG Chen-yun2, MENG Liu-wei1, LI Qing*1 (1. College of Pharmacy, Guangxi Medical University, Nanning 530021, China; 2. Department of Pharmacy, Affiliated Tumor Hospital of Guangxi Medical University, Nanning 530200, China), Huaxue Shiji, 2022, 44(6)

Abstract: Serine proteases are closely related to human life and health. Abnormal levels of serine proteases in the human body can cause diseases and endanger human life. Serine protease fluorescent probes are of great significance for detecting the number and activity dynamics of serine proteases in vivo and in vitro, as well as the treatment of clinical diseases. Therefore, this review article focuses on reviewing common serine protease fluorescent probes with excellent performance in the past five years. Based on the chromogenic labeling of various serine proteases, this review summarizes the current synthesis and performance research of fluorescent probes for serine proteases, aiming to provide a theoretical reference for the design strategies and detection applications of fluorescent probes for serine proteases.

Key words: serine protease; fluorescent probe; performance study

引用本文:尧功梅,庞承云,蒙柳卫,等. 丝氨酸蛋白酶有机小分子荧光探针的研究进展[J]. 化学试剂,2022446791-800.

 

 

基于纳米材料的比色适配体传感器的应用

韩高寰,李静*,张冰,王之飞,汤顺洁,赵志换,高文超*

(太原理工大学 生物医学工程学院,山西 太原  030024

 

摘要:比色分析是一种检测目标物的方法,具有肉眼可见、操作方便、快捷、实时等优点,被广泛应用于医疗分析、环境监测、食品安全和质量分析等领域。纳米材料具有优良的光学性能和催化性能,目前通常被当作信号转化元件应用在比色传感器中。核酸适配体(AptamerApt具有特异性识别功能且易于修饰和编辑,在比色传感器的设计中主要作为识别元件,也可以作为信号转化元件和信号放大元件。基于纳米材料的比色适配体传感器同时具备了两种材料的优点,可以实现对大多数目标物的检测,是极具潜力的比色传感器研究方向。文章总结了基于纳米材料和Apt结合的比色传感器的构建方案和显色原理,并简要归纳了其在农药、癌症标志物、生物小分子、抗生素、重金属离子等目标物检测当中的研究进展。

关键词:传感器;适配体;纳米材料;分析检测;

中图分类号:O657.3      文献标识码: A     文章编号:0258-32832022

 

Colorimetric Apta-sensors Based on Nanomaterials and Its Applications HAN Gao-huanLI Jing*ZHANG BingWANG Zhi-feiTANG Shun-jieZHAO Zhi-huan, GAO Wen-chao* (School of Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030024, China), Huaxue Shiji202244(6)

Abstract: Colorimetric analysis is an efficient method for detecting objects, it has been widely used in medical analysis, environmental monitoring, food safety, and quality analysis owing to their visible, easy/fast operation, high real-time merits, and so on. While nanomaterials have excellent optical and catalytic properties, which are often used as signal conversion components in colorimetric sensors. Aptamers have specific recognition functions, they are easy to be modified and edited, therefore have been mainly used as recognition components for designing colorimetric sensors, as well as signal conversion and amplification components. The colorimetric sensors based on the combination of nanomaterials and aptamers integrate the advantages of each component and can realize the detection of most target objects, which is one promising colorimetric sensor research area. In this review article, the construction scheme and color rendering principle of the colorimetry Apta-sensors are summarized. Furthermore, the main applications of detecting pesticides, cancer markers, biologically small molecules, antibiotics, heavy metal ions, and other target objects are also briefly summarized.

Key words: sensor; aptamer; nanomaterials; analytical detection

引用本文:韩高寰,李静,张冰,等. 基于纳米材料的比色适配体传感器的应用 [J]. 化学试剂,2022446801-809

 

 

【生化与药用试剂】

雷公藤红素与人血清白蛋白的相互作用

刘浩1樊世萌1欧阳敬禹1尤祥宇*1苏江涛1李玲玲2肖红卫3

1. 湖北工业大学 生物工程与食品学院,湖北 武汉 4300682. 武汉文理学院 医学院,湖北 武汉 4303453. 湖北省农业科学院 畜牧兽医研究所 动物胚胎工程与分子育种湖北省重点实验室,湖北 武汉 430072

 

摘要:通过使用荧光光谱、分光光度法以及等温滴定量热法等研究方法,研究了人血清白蛋白(HSA)与雷公藤红素的结合方式,采用分子对接的方式分析相互作用模式。荧光光谱结果可知,雷公藤红素与HSA主要通过氢键和范德华力结合,并且雷公藤红素猝灭HSA内源荧光的机制为静态猝灭,同时两者的结合过程主要受温度影响。在两者的结合过程中,会导致HSA的构象与微环境发生微小的改变。结合分子对接结果可知,两者的结合过程可能主要是通过疏水相互作用、范德华力等弱相互作用进行结合。为雷公藤红素在血液中的运输及传递提供了理论支持,对深入理解雷公藤红素的药效学和药代动力学性质具有重要的意义。

关键词:人血清白蛋白;雷公藤红素;荧光;等温滴定量热法;分子对接

中图分类号:R961      文献标识码:A      文章编号:0258-32832022--

 

Interaction between Celastrol and Human Serum Albumin LIU Hao1, Fan Shi-meng1, Ouyang Jing-yu1,You Xiang-yu*1, Su Jiang-tao1, Li Ling-ling2,XIAO Hong-wei3 (1.School of Food and Biological Engineering, Hubei Universityof Technology, Wuhan 430068, China; 2.Medical School, Wuhan University of Arts and Science, Wuhan 430345, China; 3. Hubei Provincial Key Laboratory of Animal Embryo Engineering and Molecular Breeding, Institute of Animal Husbandry and Veterinary Medicine, Hubei Academy of Agricultural Sciences, Wuhan 430072, China), Huaxue Shiji, 2022, 44(6),

Abstract: In this paper, fluorescence spectroscopy, spectrophotometry, and isothermal titration calorimetry were used to study the binding mode of simulated human serum albumin (HSA) and celastrol, and molecular docking was used to analyze the interaction mode. Fluorescence spectrum results showed that celastrol and HSA are mainly bound via hydrogen bond and intermolecular force, and the mechanism of celastrol quenching HSA endogenous fluorescence is static quenching, and the binding process of celastrol and HSA is mainly affected by temperature. In the combination process, it was revealed that the conformation and microenvironment of HSA will change slightly. Combining the molecular docking results, the bonding process of the two may be mainly governed by weak interactions such as hydrophobic interaction and intermolecular force. This study provides theoretical support for the transport and delivery of celastrol in blood and is of great significance for further understanding the pharmacodynamics and pharmacokinetic properties of celastrol.

Key words: human serum albumin; celastrol; fluorescence;isothermal titration calorimetry; molecular docking

引用本文:刘浩,樊世萌,欧阳敬禹,等. 雷公藤红素与人血清白蛋白的相互作用[J]. 化学试剂,2022, 446810-815.

 

 

3,5-二芳基取代吡唑为Cap的新型选择性HDAC6抑制剂:设计、合成及抑酶活性评价

何格1,张明明1,李志1,徐星星1,袁真1,王琴1,马晓东*1,2

1. 安徽中医药大学 药学院,安徽 合肥 2300382. 安徽省中医药科学院 药物化学研究所,安徽 合肥 230012

 

摘要:为发现新型组蛋白去乙酰化酶抑制剂(Histone deacetylase inhibitors, HDACis基于现有代表性选择性HDAC6抑制剂的结构特征,采用构象限制型的3, 5-二芳基取代吡唑Cap单元构建目标分子,经Claisen-Schmidt反应、环合、亲核取代、水解、缩合、羟胺解反应合成了9个化合物,并通过氢谱和质谱对其进行结构确证。抑酶活性测试结果显示,化合物4-((3,5-(4-氯苯基)-1H-吡唑-1-)甲基)-N-羟基苯甲酰胺(5aHDAC6具有良好的抑制活性(IC50 = 0.25 μmol/L)和一定的亚型选择性。

关键词:设计;合成;组蛋白去乙酰化酶6抑制剂;抑酶活性评价;选择性

中图分类号:R914.5      文献标识码A      文章编号0258-32832022--

 

Novel Selective HDAC6 Inhibitors Bearing 3, 5-Diaryl-substituted 1H-Pyrazole as Capmoiety: The Design, Synthesis and Evaluation of Enzymatic Activity HE Ge1, ZHANG Ming-ming1, LIZhi1, XU Xing-xing1, YUAN Zhen1, WANG Qin1, MA Xiao-dong*1,2 (1. College of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038, China; 2. Department of Medicinal Chemistry, Anhui Academy of Chinese Medicine, Hefei 230012, China), Huaxue Shiji, 2022, 44(6), 00 ~ 00

Abstract: This study is conducted to discover novel histone deacetylase inhibitors (HDACis). Based on the structural characteristics of the representative histone deacetylase 6 (HDAC6) selective inhibitors, nine target compounds that feature conformationally restricted 3, 5-diaryl-substituted 1H-pyrazole as the Cap moiety were designed based on structural characteristics of the representative selective HDAC6is, and synthesized via Claisen-Schmidt reaction, cyclization reaction, substitution reaction, hydrolysis, condensation with THP protected hydroxylamine and deprotection. Their molecular structures have been confirmed by 1H NMR and MS. The biochemical assay showed that compound 4-((3,5-bis(4-chlorophenyl)-1H-pyrazol-1-yl)methyl)-N-hydroxybenzamide (5a) exhibited acceptable HDAC6 inhibitory activity (IC50 = 0.25 μmol/L) and moderate selectivity.

Key words: design; synthesis; histone deacetylase 6 inhibitor; biochemical assay; selectivity

引用本文:何格,张明明,李志,等. 3,5-二芳基取代吡唑为Cap的新型选择性HDAC6抑制剂:设计、合成及抑酶活性评价[J]. 化学试剂, 2022, 44(6):816-821

 

【功能材料】

改性柚子皮生物炭吸附亚甲基蓝性能研究

张妍杰,王欢,蔡玉福,边子琦,赵兴,刘彦琳,赵永华*

(辽宁工业大学 化学与环境工程学院,辽宁 锦州  121001

 

摘要:采用硝酸-高锰酸钾活化法对制备的柚子皮生物炭进行改性处理,并将其作为吸附剂探究了其对亚甲基蓝的吸附性能。通过静态吸附实验考察了亚甲基蓝溶液的pH、初始浓度、吸附时间、吸附温度、吸附剂投加量等条件对吸附效果的影响,并确定了该吸附过程的吸附动力学、吸附等温线和吸附热力学。实验结果表明,在改性生物炭投加量为0.6 g/LpH 7、亚甲基蓝溶液浓度为100 mg/L50 oC吸附180 min的条件下,改性生物炭对亚甲基蓝的吸附容量为68.28 mg/g。通过准二级动力学方程和Freundlich方程更好的描述了该吸附过程,同时吸附热力学表明该吸附过程是一个自发吸热过程。

关键词:柚子皮;生物炭;亚甲基蓝;吸附

中图分类号X703      文献标识码A      文章编号0258-32832022

 

Adsorption of Methylene Blue by Modified Pomelo Peel Biochar ZHANG Yan-jie, WANG Huan, CAI Yu-fu, BIAN Zi-qi, ZHAO Xing, LIU Yan-lin, ZHAO Yong-hua*(School of Chemistry & Environmental Engineering, Liaoning University of Technology, Jinzhou 121001, China), Huaxue Shiji, 2022, 44(6)

Abstract: Pomelo peel-derived biochar was firstly modified by using nitric acid-potassium permanganate activation method and used as adsorbent for methylene blue (MB), the adsorption performance for methylene blue was investigated. The influences of pH, initial MB concentration, adsorption time, adsorption temperature, and the amount of adsorbent on the adsorption performance of Pomelo peel-derived biochar were investigated by static adsorption experiments, and the adsorption kinetics, adsorption isotherms, and adsorption thermodynamics were determined. The results showed that the adsorption capacity of MB was 68.28 mg/g under the condition of adsorbent concentration of 0.6 g/L, pH of 7, methylene blue concentration of 100 mg/L, and adsorption at 50 oC for 180 min. The adsorption process could be better described by the quasi-second-order kinetic equation and Freundlich equation. Adsorption thermodynamics revealed that the adsorption was spontaneous and endothermic. Key words: pomelo peel; biochar; methylene blue; adsorption

引用本文:张妍杰, 王欢, 蔡玉福, .改性柚子皮生物炭吸附亚甲基蓝性能研究[J].化学试剂, 2022, 446):822-827.

 

 

纳米零价铁吸附法去除废水中的Pb2+

左国强*,苏小莉,刘改云,宋欣宇,张露露

(济源职业技术学院 冶金化工系,河南 济源  459000

 

摘要:通过液相还原法,采用NaBH4还原Fe2+制备了粒径约为50 nm的纳米零价铁(nZVI),并应用于含Pb2+废水,详细考察了颗粒大小、酸度、温度、投入量、初始浓度和反应时间对Pb2+去除率的影响。结果表明,过量的NaBH4有利于nZVI网状结构的生成,也有利于nZVI对溶液中Pb2+的去除,常温下,调节溶液pH46nZVI的投加量为0.5 g/L,当Pb2+初始浓度小于200 mg/L时,nZVI可在20 min内完成对Pb2+的去除,当Pb2+的初始浓度为300500 mg/L时,反应时间延长至60 min才能完全去除,而当Pb2+的初始浓度为600 mg/L时,去除率最大仅为84.2%。动力学实验表明,nZVI对溶液中Pb2+的吸附符合Lagergren准二级动力学模型,其吸附过程受化学吸附控制。LangmuirFreundlich等温吸附模型对该过程的拟合程度都较高,表明Pb2+的去除过程中单分子吸附和多分子吸附共存。当Pb2+的初始浓度小于10 mg/L时,滤液中的Fe2+浓度低于生活饮用水卫生标准《GB5749—2006》中规定的限量要求,不会对环境造成二次污染。

关键词:纳米零价铁(nZVI);铅;吸附;废水;吸附动力学

中图分类号:X703     文献标识码:A     文章编号:0258-32832022

 

Research on the Removal of Pb2+ from Wastewater by Nanometer Zero-Valent Iron ZUO Guo-qiang, SU Xiao-li, LIU Gai-yun, SONG Xin-yu, ZHANG Lu-lu (Department of Metallurgy and Chemical Engineering, Jiyuan Vocational and Technical College, Jiyuan 459000, China), Huaxue Shiji, 2022, 44(6)

AbstractNanoscale zero-valent iron (nZVI) with average particle of 50 nm was synthesized in aqueous solutions by reduction of Fe2+ with NaBH4. Experiment to remove Pb2+ in solution by nZVI was carried out. The effects of particle size, pH, temperature, dosage, initial concentration and reaction time on removal efficiency of Pb2+ were investigated. The results showed that, it was beneficial to the formation of network structure and the removal of Pb2+ in the solution, when the amount of NaBH4 was in large excess. At room temperature, adjust the pH of the solution to 46, and the dosage of nZVI was 0.5 g/L, nZVI could remove Pb2+ in 20 min, while the initial Pb2+ concentration was less than 200 mg/L. However, in order to remove Pb2+ completely, the reaction time was extended to 60 min, when the initial concentration of Pb2+ is 300500 mg/L. When the initial concentration of Pb2+ was 600 mg/L, the maximum removal efficiency was only 84.2%. Kinetic experiments showed that, the adsorption kinetics of Pb2+ on nZVI in solution was in accordance with Lagergren-pseudo -second- order model, which was mainly controlled by chemical adsorption. The adsorption behavior was highly compatible with Langmuir and Freundlich isothermal adsorption models, indicating that removal of Pb2+ was monolayer adsorption coexisting with multi-layer adsorption. When the initial Pb2+ concentration was less than 10 mg/L, the concentration of Fe2+ in the filtrate was lower than the limited demand of Standards for Drinking Water Quality GB5749—2006, which would not cause secondary pollution to the environment.

Key wordsnanoscale zero-valent iron (nZVI); Pb; adsorption; wastewateradsorption kinetic

引用本文:左国强,苏小莉,刘改云,等. 纳米零价铁吸附法去除废水中的Pb2+[J]. 化学试剂, 2022, 44(6): 828-834

 

 

氯化铁改性椰壳活性炭去除2,4-二氯苯酚的吸附性能研究

刘雪平,闫晓乐,张焕,张瀚月,田丽,宋忠贤,毛艳丽,张霞,延旭,康海彦*

(河南城建学院 河南省水体污染与防治重点实验室,河南平 顶山  467000

 

摘要以椰壳活性炭为原料,进行氯化铁改性,探究其对2,4-二氯苯酚吸附性能影响的研究。通过静态吸附实验得到了最佳改性条件,使得2,4-二氯苯酚吸附性能进一步得到提升,并结合实际水体酸碱性探究,对模拟废水实验进行了pH探究,进一步优化了材料对实际水体的适用性。研究表明,氯化铁浓度为0.8mol/L、改性时间为24h条件下改性得到的炭材料(BC-F)吸附性能最佳;吸附剂的最佳使用量应为0.04g吸附过程应在弱酸或碱性环境中进行,在实际水体中实用性较好;且该吸附过程符合准一级动力学和Freundlich等温吸附方程,以化学吸附为主。

关键词椰壳活性炭;氯化铁改性;吸附;2,4-二氯苯酚;动力学

中图分类号:X703        文献标识码:A            文章编号:0258-32832022- -

 

Adsorption Performance of FeCl3 Modified Coconut Shell Activated Carbon for the Removal of 2,4-Dichlorophenol LIU Xue-ping, YAN Xiao-le, ZHANG Huan, ZHANG Han-yue, TIAN Li, SONG Zhong-xian, MAO Yan-li, ZHANG Xia, YAN Xu, KANG Hai-yan*Henan Key Laboratory of Water Pollution Control and Rehabilitation, Henan University of Urban Construction, Pingdingshan 467000, China, Huaxue Shiji, 2022, 44(6),

Abstract: In this study, ferric chloride-modified coconut shell-derived activated carbon (AC) was prepared, the effect of ferric chloride modification on the adsorption performance of 2,4-dichlorophenol was investigated. The optimum modification conditions were obtained through static adsorption experiments, which significantly improved the adsorption performance of 2,4-dichlorophenol. The pH of the simulated wastewater experiment was also investigated in combination with the acidity and alkalinity of actual wastewater to further optimize the applicability of the as-modified material. This study presented that the best adsorption performance of ferric chloride-modified AC was obtained with a dosage of 0.8 mol/L ferric chloride concentration and a modification time of 24 h; also, the adsorption process is suggested to be carried out in a weakly acidic or alkaline environment, which is close to the practical condition in the actual wastewater. Furthermore, the adsorption process was testified to conform to the quasi-level kinetics and Freundlich isothermal adsorption equation that was governed by chemisorption.

Key words: coconut shell activated carbon; FeCl3 modified; adsorption; 2,4-DCP; Kinetics

引用本文刘雪平,闫晓乐,张焕,等. 氯化铁改性椰壳活性炭去除2,4-二氯苯酚的吸附性能研究[J]. 化学试剂,202244(6):835-840

 

 

板栗壳活性炭对中性红和活性蓝19的吸附行为

韦琴*,周帆

(武汉工商学院 环境与生物工程学院,湖北 武汉  430065

 

摘要:以板栗壳为原料制备板栗壳活性炭,以振荡时间、pH和温度3个单因素考察了板栗壳活性炭对中性红和活性蓝19的吸附效果,分析了等温吸附过程并从吸附动力学角度探讨了两种染料的吸附机理。结果表明:板栗壳活性炭对中性红染料的最佳吸附条件是pH 4、温度为35 ℃,振荡时间为120 min;对活性蓝19最佳吸附条件是pH 2、温度为40 ℃,振荡时间为150 min。板栗壳活性炭对两种染料的吸附过程与Freundlich模型拟合度更高,该过程主要是多分子层吸附。用准二级动力学方程(R20. 99)比准一级动力学方程更适合描述板栗壳活性炭对两种染料的吸附特性。板栗壳活性炭对两种染料的吸附以化学吸附为主。

关键词板栗壳活性炭;中性红;活性蓝19;吸附行为;Freundlich模型

中图分类号:TQ0      文献标识码:A      文章编号:0258-32832022--

 

Adsorption Behavior of Chestnut Shell Activated Carbon for Neutral red and Active Blue 19 WEI Qin*, ZHOU Fan (College of Environmental and Biological Engineering, Wuhan Technology and Business University, Wuhan 430065, China), Huaxue Shiji, 2022, 44(6),

Abstract: Herein, activated carbon (AC) was prepared from the chestnut shell. The effect of chestnut shell-derived AC on the adsorption of neutral red and active blue 19 was explored by varying the following parameters including oscillation time, pH, and temperature. The isothermal adsorption process was analyzed and the mechanism for adsorbing the two dyes was discussed from the viewpoint of adsorption kinetics. Results showed that the optimal adsorption conditions for neutral red dye were pH of 4.0, the temperature of 35 ℃, and the oscillation time of 120 min. The optimum adsorption conditions for active blue 19 were pH of 2.0, the temperature of 40 ℃, and the oscillation time of 150 min. The adsorption processes of the two dyes on chestnut shell-derived AC matched better with the Freundlich model, indicating that the process was governed by multi-molecular layer adsorption. Furthermore, the quasi-second-order kinetic equation (R2>0.99) was more suitable than the quasi-first-order kinetic equation to describe the adsorption characteristics, suggesting that these two dyes were chemically adsorbed on chestnut shell-derived AC.

Key words: chestnut shell activated carbon; neutral red; activated blue 19; the adsorption behavior; Freundlich model

引用本文:韦琴,周帆. 板栗壳活性炭对中性红和活性蓝19的吸附行为[J]. 化学试剂,202244(6): 841-845

 

 

CdI2-phen/bpy溶剂热体系中Cd(II)配合物的合成、晶体结构及荧光传感性能研究

朱圣加,陈飞,张柔,付玉,许伟*,罗云杰

(宁波大学 材料科学与化学工程学院,浙江 宁波  315211)

 

摘要:在溶剂热条件下,利用CdI2分别与邻菲啰啉(phen)、2,2-联吡啶(bpy)反应得两例新的Cd配合物Cd(phen)2I2Cd(bpy)2I2。通过X-射线单晶衍射、红外光谱、热重分析等方法对其表征。晶体结构分析表明,Cd(II)离子与两个phenbpy配体上4N原子以及2I原子配位形成畸变的八面体配位,借助π-π堆积和CH···I氢键相互作用形成超分子构筑。此外,还研究了配合物Cd(phen)2I2 对不同金属阳离子的荧光传感性能,结果表明Fe3+具有出较高选择性和明显的荧光猝灭响应。

关键词:镉(II)配合物;晶体结构;荧光传感;Fe3+

中图分类号:O652.3        文献标识码:A       文章编号:0258-32832022

 

Synthesis, Crystal Structure and Fluorescence Sensing Properties of Cd(II) Complex in CdI2 -phen/bpy Solvothermal System ZHU Sheng-jia, CHEN Fei, ZHANG Rou, FU Yu, XU Wei*, LUO Yun-jie (School of Material Science Chemical Engineering, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2022

446

AbstractTwo new Cd complexes: Cd(phen)2I2 and Cd(bpy)2I2 were prepared under solvothermal conditions by reacting CdI2 with 1,10-phenoline (phen) and 2,2 '-bipyridine (bpy), respectively. The complexes were characterized by using IR, TG, and X-ray single crystal diffraction. The crystal structure analysis revealed that each Cd(Ⅱ) ion is coordinated with four N atoms from the two phen or bpy ligands, and two I atoms are forming a distorted octahedral coordination geometry. The supramolecule was constructed via π-π stacking and CH··I hydrogen bond interactions. The fluorescent sensing of complex 1 to a series of metal cations was investigated. The results showed that Fe3+ ion had higher selectivity and apparent fluorescence quenching response.

Key wordsCd(II) complex; crystal structure; fluorescent sensing; Fe3+

引用本文:朱圣加,陈飞,张柔,等. CdI2-phen/bpy溶剂热体系中Cd(II)配合物的合成、晶体结构及荧光传感性能研究[J]. 化学试剂,2022446846-849.

 

 

铜滤膜基环丙沙星分子印迹复合膜的制备、吸附性能及SERS活性研究

张杰a,唐丽a,卜明a,马玉坤b,王海君*a,王静a

(齐齐哈尔医学院 a.药学院,b.医药科学研究院,黑龙江 齐齐哈尔  161006)

 

摘要:为实现环丙沙星的快速识别,制备了可以选择性吸附环丙沙星的具有表面增强拉曼活性的铜滤膜基分子印迹复合膜。以环丙沙星为模板分子,铜滤膜为基膜,甲基丙烯酸为功能单体,乙二醇二甲基丙酸酯为交联剂,偶氮二异丁腈为引发剂,甲醇、二氯甲烷的混合溶剂为反应溶剂和致孔剂,通过自由基聚合制备了分子印迹复合膜。红外光谱表征膜的结构,显微镜表征膜的形貌。对膜的吸附性能和表面增强拉曼散射活性进行了系统研究。复合膜为一层白色、连续、均匀的薄膜,表面光滑无裂纹。120 min左右膜对环丙沙星的吸附达到平衡,最大吸附量为8.11 μg/cm2,至少可以重复使用6次,印迹因子为4.0。膜具有表面增强拉曼散射活性,对环丙沙星检测的最低浓度为1.00×10-8 mol/L

关键词:环丙沙星;分子印迹;复合膜;铜滤膜;表面增强拉曼散射

中图分类号:O657.1      文献标识码:A      文章编号:0258-32832022--

 

Preparation and Adsorption Properties of Ciprofloxacin Molecularly Imprinted Composite Membrane with SERS Activity based on Copper Filter Membrane ZHANG Jiea, TANG Lia, BU Ming a, MA Yu-kun b, WANG Hai-jun*a, WANG Jing a (a.College of Pharmacy; b. Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Heilongjiang Qiqihar 161006), Huaxue Shiji, 2022, 44(6),

Abstract: In order to realize the rapid recognition of ciprofloxacin (CIP), a molecularly imprinted composite membrane (RC-MIM) with Surface-Enhanced Raman Scattering (SERS) activity based on copper filter membrane was prepared, which could selectively absorb CIP. Using CIP as the template molecule, copper filter membrane as the base membrane, methacrylic acid (MAA) as the functional monomer, and ethylene glycol dimethylpropionate (EGDMA) as the crosslinking agent, azodiisobutyronitrile (AIBN) as the initiator, mixed solvent (methanol and dichloromethane) respectively as the reaction solvent and porogen, RC-MIM was prepared via free radical polymerization. The structure of the RC-MIM was characterized by infrared spectroscopy and the morphology by optical microscope. The adsorption performance and SERS activity of the membrane were systematically studied, revealing that RC-MIM was a white, continuous, and uniform membrane with a smooth surface and free of crack. The adsorption of ciprofloxacin on the membrane reached equilibrium after about 120 min, and the maximum adsorption capacity was 8.11 μg/cm2. The membrane could be reused at least 6 times, and the imprinting factor was 4.0. Due to the SERS activity of RC-MIM, the minimum detection concentration of ciprofloxacin was 1.00×10-8 mol/L.

Key words: ciprofloxacin; molecularly imprinted; composite membrane; copper filter membrane; Surface-Enhanced Raman Scattering

引用本文:张杰,唐丽,卜明,等. 铜滤膜基环丙沙星分子印迹复合膜的制备、吸附性能及表面增强拉曼散射活性研究[J]. 化学试剂,2022446850-857.

 

 

过渡金属取代磷钼酸催化剂的制备及氧化脱硫性能研究

高爽,张俊茹,李佳其,于悦,韩璐,肖舒宁,袁运鸿,陈晓陆*

(营口理工学院 化学与环境工程学院 辽宁省化学助剂合成与分离重点实验室,辽宁 营口  115014

 

摘要:以有机氨功能化的SBA-15为载体,制备过渡金属取代的磷钼酸PMo11M, M = Fe, Co, Cu)负载型催化剂。利用XRDFT-IRBETTEMTG等手段对催化剂结构进行表征,结果表明,过渡金属成功负载到载体SBA-15上;催化剂的整体结构没有发生明显改变,催化剂活性组分均匀地分散在介孔SBA-15的表面和孔道中。结合XPS数据和氧化脱硫实验结果,发现催化剂表面的氧空位,可以活化活性氧物种,有助于催化剂脱硫性能的提升。以二苯并噻吩(DBT)为底物,进行氧化脱硫反应,考察引入的过渡金属对催化剂结构的改变和催化活性的影响。得到Co取代催化剂(PMo11Co-NH2-SBA-15)的脱硫效果最好,DBT的转化率达到91.15%PMo11Co-NH2-SBA-15催化剂具有良好的循环稳定性。

关键词:过渡金属;氧化脱硫;SBA-15;磷钼酸;二苯并噻吩

中图分类号:O643.3            文献标识码:A    文章编号:0258-32832022

 

Preparation of Transition Metal Substituted Phosphomolybdic Acid and Catalytic Performance in Oxidation Desulfurization GAO Shuang, ZHANG Jun-ru, LI Jia-qi, YU Yue, HAN Lu, XIAO Shu-ning, YUAN Yun-hong, CHEN Xiao-lu* (Liaoning Key Laboratory of Chemical Additive Synthesis and Separation, Department of Chemical Engineering, Yingkou Institute of Technology, Yingkou 115014, China), Huaxue Shiji, 2022, 44(6)

AbstractThe supported catalysts of transition metal-substituted phosphomolybdic acid (PMo11M, M = Fe, Co, Cu) were prepared using organic ammonia-modified SBA-15 substrate. The as-made catalysts were characterized by using XRD, FT-IR, BET, TEM, and TG. Results showed that the transition metals have been successfully loaded on the organic ammonia-modified SBA-15 support. The overall structure of the catalyst has not changed apparently, and the active components of the catalyst were uniformly distributed on the surfaces of mesopores of SBA-15. Combined with XPS data and oxidative desulfurization experimental results, it was found that the oxygen vacancy on the catalyst surface can efficiently generate active oxygen species, which is helpful to improve the desulfurization performance. The oxidative desulfurization reaction was carried out with dibenzothiophene (DBT) as a substrate. The effects of transition metals on the structure and catalytic activity of the catalysts were investigated. It was found that the PMo11Co-NH2-SBA-15 catalyst possessed the best desulfurization performance, achieving a conversion of 91.15% for DBT and very good cycling stability.

Key words: transition metal; oxidation desulfurization; SBA-15; phosphomolybdic acid; dibenzothiophene

引用本文:高爽,张俊茹,李佳其,等. 过渡金属取代磷钼酸催化剂的制备及氧化脱硫性能研究[J]. 化学试剂, 2022, 44(6): 858-864

 

 

【分离提取技术】

正交试验法优化复方玉液汤提取工艺及对小鼠的急性毒性研究

张文祥,郭凤,陈鹏德,吴思宇,姚蓝*

(新疆医科大学 中医学院,新疆 乌鲁木齐  830057

 

摘要:优化玉液汤的提取工艺并考察其对小鼠的急性毒性。通过设置3个考察因素:料液比、药材浸泡时间、提取时间,确立3个评价指标:总皂苷含量、干膏得率、总多糖含量。在此基础上设计正交试验并根据综合评分结果确定玉液汤的最佳提取工艺。按此提取工艺对玉液汤进行回流提取,所得药液进行小鼠的急性毒性研究。小鼠给药后连续观察14 d,在此期间内记录小鼠的基本状态、检测各组小鼠血常规和生化指标;取小鼠心、肝、脾、肺、肾计算脏器指数,HE染色观察各组小鼠脏器病理变化。最终确定玉液汤水提工艺最佳条件为:料液比 110g/L)、药材浸泡1 h、回流 2.5 h。小鼠连续给药14 d内未出现中毒和死亡情况,且给药组与对照组比较,体质量、摄食量、摄水量、血常规、生化指标和各脏器的脏器指数均未有统计学差异;各组小鼠主要脏器病理学未见异常。优化条件下的玉液汤水提工艺含量稳定,且服用安全无毒。

关键词:玉液汤;水提工艺;急性毒性;总皂苷;干膏得率;总多糖;

中图分类号:R284.2    文献标识码:A    文章编号:0258-3283202107

 

Orthogonal Experiment of Optimizing the Extraction Process of Compound Yuye Decoction and Study on Its Acute Toxicity to Mice ZHANG Wenxiang, GUO Feng, CHEN Pengde, WU Siyu, YAO Lan (College of Traditional Chinese Medicine, Xinjiang Medical University, Urumqi 830057, China) Huaxue Shiji, 2021, 44(6)

Abstract: The objective of this work is to optimize the extraction process of nectar soup and explore its acute toxicity on mice. Methods include studying the liquid/material ratio, the soaking time of medicinal herbs, and the extracting time. The evaluation factor of this study is the content of total saponins, the dry ointment yield, total polysaccharide content. The best extraction process of nectar soup was obtained based on the design of an orthogonal experiment. Reflux extraction of Yuye decoction was carried out according to the abovementioned extraction process, and the acute toxicity of the solution was studied using mice. The mice were observed for 14 days after administration. During this period, the basic state of the mice, blood routine, and biochemical indexes of each group were recorded. The heart, liver, spleen, lung, and kidney of mice were collected to calculate the viscera index, and the pathological changes of viscera were observed by HE staining. Results indicated that the optimal extraction conditions of Yuye decoction were the solid-liquid ratio of 1:10, soaking for 1h, and reflux for 2.5 h. No poisoning or death of mice occurred within 14 days of continuous administration, meanwhile, there were no statistically significant differences in body weight, food intake, water intake, blood routine, biochemical indexes, and organ indexes between the administration group and the control group. No abnormality was found in the pathology of the main organs in each group. In conclusion, the content of Yuye decoction is stable and safe under our optimized conditions.

Key words: Yuye decoction; water extraction process; acute toxicitytotal saponin dry paste yieldtotal polysaccharides;

引用本文:张文祥,郭凤,陈鹏德,等. 正交实验法优化复方玉液汤提取工艺及对小鼠的急性毒性研究[J]. 化学试剂, 2022, 44(6): 865-871

 

 

【电化学和新能源】

基于石墨烯金粒子的肾上腺素分子印迹电化学传感器研究

孙晨阳,康天放*,鲁理平,程水源

(北京工业大学 区域大气复合污染防治北京市重点实验室 环境与生命学部,北京  100124)

 

摘要:制备了石墨烯和金纳米粒子的复合物(GS-AuNP),用扫描电镜对其进行了表征。将该复合物和壳聚糖(CS)依次修饰到玻碳电极(GCE)表面,制得修饰电极(CS/GS-AuNP/GCE)。以3-氨基苯硼酸盐酸盐(APBA)为单体,肾上腺素(EP)分子为模板,采用循环伏安法在该修饰电极表面进行电聚合,制备了分子印迹聚合物(MIP)膜,洗脱掉模板分子EP后得到分子印迹传感器(MIP/CS/GS-AuNP/GCE),用于肾上腺素的检测。溶液中的EP可与传感器表面的MIP特异性结合,在富集一定时间后,通过差分脉冲伏安法(DPV)检测溶液中EP的浓度。在优化的实验条件下,DPV峰电流分别在1.0×10-71.0 × 10-5 mol/L1.0 ×10-51.0 × 10-4 mol/L EP的浓度范围内随EP浓度的增大而呈线性增大,检出限为5×10-8 mol/L制备的MIP/CS/GS-AuNP/GCE传感器成功应用于实际样品中的肾上腺素含量检测,回收率在98%105%之间。

关键词:GS-AuNP复合物;电化学传感器;分子印迹聚合物;电聚合;肾上腺素

 

Molecularly Imprinted Electrochemical Sensor for Epinephrine Based on the Composite of Graphene and Gold Particles SUN Chen-yang, KANG Tian-fang*, LU Li-ping, CHENG Shui-yuan ( Key Laboratory of Beijing on Regional Air Pollution Control, Faculty of Environment and Life, Beijing University of Technology, Beijing 100124, China), Huaxue Shiji , 2022 , 44(6)

Abstract: The composite of the graphene sheet (GS) and gold nanoparticles (AuNP) was prepared and characterized by using scanning electron microscope. The as-made composite and chitosan (CS) were modified onto the surface of a glassy carbon electrode in sequence to prepare a modified electrode (denoted as CS/GS-AuNP/GCE). Using 3-aminophenylboratic acid (APBA) as monomer and epinephrine (EP) molecules as a template, electropolymerization was carried out on the surface of the modified electrode by cyclic voltammetry. After eluting the template EP, the molecularly imprinted electrochemical sensor (MIP/CS/GS-AuNP/GCE) was obtained. EP can specifically bind to the MIP on the surface of the sensor. After a certain period of enrichment, the concentration of EP in the solution can be detected by differential pulse voltammetry (DPV). Under optimized experimental conditions, the DPV peak current increased linearly with the increase of EP concentration in the ranges of 1.0 × 10-7 ~ 1.0 × 10-5 mol/L and 1.0 × 10-5 ~ 1.0 × 10-4 mol/L. The detection limit is 5×10-8 mol/L. In conclusion, the MIP/CS/GS-AuNP/GCE sensor was successfully applied to the detection of EP in actual samples with a good recovery rate of 99.9% to 104.7%.

Key wordsGS-AuNP composite; electrochemical sensor; molecularly imprinted polymer; electropolymerization; epinephrine

引用本文:孙晨阳,康天放,鲁理平,等. 基于石墨烯金粒子的肾上腺素分子印迹电化学传感器研究 [J]. 化学试剂, 2022, 44(6) :872-879

 

 

茜素绿染料的Ti/PbO2电极与Ti/IrO2+Ta2O5电极催化降解比较研究

 

沈宏*1章维维2姚春冀1杨叶1范宏亮1,鞠莉1

1. 杭州医学院公共卫生学院,浙江 杭州 3100072. 杭州嘉澍环境监测有限公司,浙江 杭州 311000

 

摘要:主要研究了Ti/PbO2电极与Ti/IrO2+Ta2O5电极催化氧化体系对茜素绿(AG)染料废水的催化降解效果。结果表明,当AG初始浓度100 mg/L,电解质浓度0.1 mol/L,电流密度30 mA/cm2pH5.86,处理70 min后,Ti/PbO2电极和Ti/IrO2+Ta2O5电极催化氧化体系对AG和化学需氧量(COD)的处理效率分别可高于81.4%51.6%。相较于Ti/IrO2+Ta2O5电极,具有四棱锥形结构晶粒的Ti/PbO2电极稳定性较高,且Ti/IrO2+Ta2O5电极表面由于存在干泥状裂痕结构,工作过程中易出现表面局部剥落现象,形成的TiO2钝化膜则会导致槽压升高和电极活性下降,影响体系的催化氧化效率。

关键词:形稳电极(DSA);Ti/PbO2电极;Ti/IrO2+Ta2O5电极;茜素绿;电催化降解

中图分类号:O643.3      文献标识码:A      文章编号:0258-32832022--

 

Degradation of Alizarin Green (AG) by Ti/PbO2 Electrode and Ti/IrO2+Ta2O5 Electrode SHEN Hong*1, ZHANG Wei-wei2, YAO Chun-ji1, YANG Ye1, FAN Hong-liang1, JU Li1(1. College of Public Health, Hangzhou Medical College, Hangzhou 310007, China; 2. Hangzhou Jiashu Environmental Monitoring Co., Ltd., Hangzhou 311000, China), Huaxue Shiji, 2022, 44(6),

Abstract: In this work, the degradation efficiencies of alizarin green (AG) by Ti/PbO2 electrode and Ti/IrO2+Ta2O5 electrode were studied. The optimal degradation conditions were obtained: initial AG concentrations of 100 mg/L, Na2SO4 concentrations of 0.1 mol/L, the current density of 30 mA/cm2, and pH of 5.86. After being treated under this specific optimal condition for 70 min, the removal rates of AG and COD were higher than 81.4% and 51.6%, respectively. Compared with Ti/IrO2+Ta2O5 electrode with a mud-cracked surface, the Ti/PbO2 electrode possessed higher stability due to its pyramid crystal structure. Because of the surface spalling phenomenon observed during the degradation experiments, passivated TiO2 film was formed, leading to the increase of cell voltage and degraded electrocatalytic oxidation capability.

Key words: dimensionally stable anode (DSA); Ti/PbO2 electrode; Ti/IrO2+Ta2O5 electrode; alizarin green (AG); electrocatalytic degradation

引用本文:沈宏,章维维,姚春冀,等. 茜素绿染料的Ti/PbO2电极与Ti/IrO2+Ta2O5电极催化降解比较研究[J]. 化学试剂,2022446):880-887.

 

 

基于Nafion/GSH-Fe3O4@Cs/Pt/GCE检测丙烯酰胺

尚平*1,杨永2,赵荣敏1,崔文广3

1. 石家庄职业技术学院 食品与药品工程系,河北 石家庄  0500812. 石家庄职业技术学院 学生工作部,河北 石家庄  0500813. 石家庄学院 化工学院,河北 石家庄  050035

 

摘要:制备Nafion/还原性谷胱甘肽-四氧化三铁@//玻碳电极(Nafion/Glutathione-ferric oxide@Carbon/ Platinum/Glassy carbon electrode, Nafion/GSH-Fe3O4@Cs/Pt/GCE)传感器,对丙烯酰胺(Acrylamide, AM)进行定量分析。合成了核壳结构的四氧化三铁@碳纳米复合材料(Ferric oxide@Carbon nanocomposites, Fe3O4@Cs),并在此基础上负载铂纳米粒子(Platinum nanoparticles, Pt),制备新型的Fe3O4@Cs/Pt纳米复合材料。以还原性谷胱甘肽(Glutathione, GSH)为探针,在Fe3O4@Cs/Pt的基础上,制备了Nafion/GSH-Fe3O4@Cs/Pt/GCE传感器。通过对GSH固载量、Nafion浓度、加成时间、加成温度等条件的优化确定传感器的最佳工作条件。研究发现,Fe3O4@Cs/Pt具有良好的导电性和生物相容性,能有效提高传感器的灵敏度;AM浓度负对数与其与GSH间加成率在1×10-101×10-5 mol/L呈良好的线性关系,线性方程为Y =     -6.025X + 73.632(XAM浓度的负对数)R2=0.9974,检出限为5.624×10-11 mol/L,且该传感器短期稳定性较好。该方法简单、方便可用于丙烯酰胺的定量分析。

关键词:纳米粒子;还原性谷胱甘肽;丙烯酰胺;传感器;检测

中图分类号:TS207.7   文献标识码:A     文章编号:0258-32832022

 

Detection of Acrylamide Based on Nafion/GSH-Fe3O4@Cs/Pt/GCE SHANG Ping*1, YANG Yong2, ZHAO Rong-min1, CUI Wen-guang3 (1. Department of Food and Drug Engineering, Shijiazhuang University of Applied Technology, Shijiazhuang 050081, China; 2.Department of Student Affairs, Shijiazhuang University of Applied Technology, Shijiazhuang 050081, China; 3.College of Chemical Engineering, Shijiazhuang University, Shijiazhuang 050035, China), Huaxue Shiji, 2022, 44 (6)

Abstract: Nafion/Glutathione-Ferric oxide@carbon/Platinum/Glassy carbon electrode, (Nafion/GSH-Fe3O4@Cs/Pt/GCE) sensor was prepared for the quantitative analysis of acrylamide (AM). Platinum nanoparticles (Pt) were loaded onto the core-shell structured Fe3O4@Cs nanocomposites to obtain the Fe3O4@Cs/Pt composites. Afterward, the Nafion/GSH-Fe3O4@Cs/Pt/GCE sensor was prepared based on Fe3O4@Cs/Pt using glutathione (GSH) as a probe molecule. The optimum working conditions of the as-made sensor were determined by optimizing the parameters such as the fixed GSH loading, Nafion concentration, addition time, and addition temperature, et al. The results showed that the Fe3O4@Cs/Pt had a good conductivity and biocompatibility, thus could effectively improve the sensor sensitivity. A good linear relationship between the negative logarithm of AM concentration and its addition rate with GSH was obtained in a range of 1×10-10 ~ 1×10-5 mol/L, the linear equation was Y=-6.025X+73.632 (X was the negative logarithm of AM concentration), R2= 0.9974, and the detection limit was 5.624×10-11 mol/L. The sensor also showed very good stability in the short term. Our method is simple and convenient and can be used for the quantitative analysis of acrylamide.

Key words: nanoparticles; glutathione; acrylamide; sensor; detection

引用本文:尚平,杨永,赵荣敏,等. 基于Nafion/GSH-Fe3O4@Cs/Pt/GCE检测丙烯酰胺[J]. 化学试剂,2022446888-893

 

 

【分析与测试】

醇类香料单体在加热卷烟中的转移行为研究

徐如彦1,朱梦薇2,饶先立1,王鸣1,胡玉轩1,李朝建1,师东方1,石怀斌1,郑晓云*1

(1. 江苏中烟工业有限责任公司,江苏 南京  2100192. 郑州轻工业大学 食品与生物工程学院,河南  郑州 450002)

 

摘要:为研究醇类香料单体在加热卷烟中的转移规律,将28种醇类香料单体添加到加热卷烟烟芯中,建立了加热卷烟烟芯中醇类香料单体的检测分析方法,并分析了醇类香料单体在加热卷烟抽吸前后的转移行为。结果显示:贮存期间,28种醇类香料单体的烟芯持留率为7.13%91.70%、降温段迁移率为09.10%、滤嘴迁移率为030.76%、散失率为1.83%81.65%。抽吸过程中,28种醇类香料单体的主流烟气粒相物转移率为2.29%34.02%、烟芯残留率为1.17%24.01%、滤嘴截留率为8.27%29.46%互为同系物的醇类单体遵守随着分子量增大、沸点增高,烟芯持留率、向主流烟气粒相物转移率增加,散失率减小的规律。互为同分异构体的醇类单体遵循物质结构稳定性越好、沸点越高,烟芯持留率和向主流烟气粒相物转移率越高,散失率越小的规律。香叶醇、橙花醇、肉桂醇的烟芯持留率高、散失率小、向主流烟气粒相物转移率高,适用做加热卷烟香精调配香原料。

关键词:电加热卷烟;醇类香料;持留率;迁移率;转移率;截留率;散失率

中图分类号:TS411                文献标识码:A     文章编号:0258-32832022

 

Study on Transfer Behavior of Alcohol Flavor Monomers in Heated Cigarettes XU Ru-yan1, ZHU Meng-wei2, RAO Xian-li1, WAN Ming1, HU Yu-xuan1, LI Chao-jian1, SHI Dong-fang1, SHI Huai-bin1, ZHENG Xiao-yun*1 (1. China Tobacco Jiangsu Industrial Co., Ltd., Nanjing 210019, China; 2. College of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002, China), Huaxue Shiji , 2022 , 44(6)

Abstract: In order to study the transfer principle of alcohol flavor monomers in heated cigarettes, 28 kinds of alcohol flavor monomers were added into heated cigarette cores, and a method for the detection and analysis of alcohol flavor monomers in heated cigarette cores was established. The transfer behavior of alcohol flavor monomers before and after smoking was analyzed. Results showed that during the storage period, the retention rate of the cigarette core of 28 kinds of alcohol flavor monomers was 7.13%~91.70%, the mobility of the cooling section was 0~9.10%, the mobility of the filter rod was 0~30.76%, and the loss rate was 1.83%~81.65%. During the smoking process, the mainstream smoke particle-phase transfer rate of 28 alcohol flavor monomers was 2.29%~34.02%, the residual rate of cigarette core was 1.17%~24.01%, and the rejection rate of filter rod was 8.27%~29.46%. Alcohol monomers that are homologous to each other obey the law that with the increase of the molecular weight and the boiling point, the retention rate of the smoke core and the rate of transferring to the mainstream smoke particle-phase matter increase, while the loss rate decreases. Alcohol monomers that are isomers of each other follow the principle that the better the stability of the material structure and the higher the boiling point, the higher the retention rate of the smoke core and the transfer rate of particulate matter to the mainstream smoke will be, also the smaller the loss rate. As revealed by our study, the geraniol, nerol, and cinnamyl alcohols have relatively high core retention rates, low loss rates, high transfer rates to mainstream smoke particles, and are suitable choices for heating cigarette flavoring and flavoring raw materials.

Key wordsheat-not-burn productalcohol spicesretention ratemobility ratetransfer raterejection rateloss rate

引用本文:徐如彦,朱梦薇,饶先立,等. 醇类香料单体在加热卷烟中的转移行为研究[J]. 化学试剂,2022446894-903

 

 

HPLC测定人血清中三种抗HIV

龚爱琴

(扬州工业职业技术学院 化学工程学院,江苏 扬州  225127

摘要:建立一种用高效液相色谱法同时测定人血清中三种抗HIV药(拉米夫定、富马酸替诺福韦二吡呋酯和ACC007)的新方法。测定时采用Dionex C185 µm4.60 mm×250 mm)色谱柱;流动相为甲醇:水,采用梯度洗脱方式,流速为0.6 mL/min;检测波长为260 nm。结果发现在优化色谱条件下,拉米夫定、富马酸替诺福韦二吡呋酯和ACC007的线性范围分别为2.07103.55.15206.02.0651.45 μg/mL,检出限分别为1.052.601.03 μg/mL,加样回收率分别为98.54%103.8%98.29%102.5%101.7%108.4%。本方法简单快速,可用于人血清中三种药物含量的测定。

关键词:抗 HIV药;拉米夫定;富马酸替诺福韦二吡呋酯;ACC007HPLC

中图分类号:O657.7       文献标识码:A      文章编码0258-32832022--

 

Simultaneous Determination of Three Anti HIV Drugs in Serum by HPLC GONG Ai-qin (Chemical Engineering Institute, Yangzhou Polytechnic Institute, Yangzhou 225127, China), Huaxue Shiji202144(6) ~

Abstract: In this work, a new method for the simultaneous determination of lamivudine, tenofovir disoproxil fumarate, and ACC007 in human serum was developed with high-performance liquid chromatography (HPLC). A Dionex C18 chromatographic column (5 µm, 4.60 mm*250 mm) was used with the methanol-water mobile phase (gradient elution) and a flow rate of the mobile phase of 0.60 mL/min. The detection wavelength was 260 nm. Under the optimized chromatographic conditions: the linear ranges of lamivudine, tenofovir disoproxil fumarate and ACC007 were 2.07 ~ 103.5, 5.15 ~ 206.0, 2.06 ~ 51.45 μg/mL, respectively; the detection limits for lamivudine, tenofovir disoproxil fumarate and ACC007 were 1.05, 2.60, and 1.03 μg/mL, respectively; and accordingly, the recoveries in the spiked samples were 98.54%~103.8%, 98.29%~102.5%, and 101.7%`108.4%, respectively. The proposed method is simple and fast and can be used for the determination of these three drugs in human serum.

Key words: Anti HIV drug, lamivudine, tenofovir disoproxil fumarate, ACC007, HPLC

引用本文:龚爱琴. HPLC测定人血清中三种抗HIV [J]. 化学试剂, 2022, 44(6): 904-907

 

 

中缅管输进口原油微量元素分析研究

 

李秀林1,韩家曦2,刘汗青1,武梦琦1,王群威3,杨新周*4

(1.  瑞丽海关,云南 瑞丽  6786002. 瑞丽中检检验认证有限公司,云南 瑞丽  6786003. 宁波海关技术中心,浙江 宁波  3150104. 德宏师范高等专科学校 理工学院,云南 芒市  678400

 

摘要:测定中缅管输原油中9种元素,为原油国别鉴定、原油溯源提供依据,为中缅管输原油运输及下游的冶炼过程提供科学基础。采用灰化碱熔-电感耦合等离子体发射光谱法对中缅管输原油中9种元素进行测定。结果表明,中缅管输进口5个国家的原油中含有AlSiVNiFeNaCaZn 8种元素,原油中均未检出P元素。8种元素中Fe含量占比75.73%V含量占比10.87%Si含量占比4.73%Ni含量占比4.18%,其余元素占比4.56%。通过分析得出,中缅管输进口的5国原油Si/VNi/V比值均小于1,呈现出海相原油的特性,不同油种元素的含量存在一定差异,且有一定的规律性,各油种间Ni/VSi/V比值相差不大,Fe/V比值的波动较大,可以按此来对5个国家原油进行溯源。

关键词:灰化碱溶;电感耦合等离子体发射光谱法;中缅管输原油;元素

中图分类号O657.3      文献标识码 A      文章编号:0258-32832022

 

Analysis of Trace Elements in Crude Oil Imported from China-Burma Pipeline LI Xiu-lin1, HAN Jia-xi2, LIU Han-qing1, WU Meng-qi1, WANG Qun-wei3YANG Xin-zhou *4 (1. Ruili Customs, Ruili 678600, China; 2.Ruili Inspection and Certification Co, LTD, Ruili 678600, China; 3. Ningbo Customs Technology Center, Ningbo, Zhejiang 315010; 4.Dehong Teachers College College of Science and Technology, Mangshi 678400, China), Huaxue Shiji, 2022, 44(6)

Abstract: The determination of nine elements in crude oil transported by China-Myanmar pipeline provides a basis for crude oil identification and traceability, and provides a scientific basis for crude oil transportation and downstream smelting process. Nine elements in crude oil from China-Myanmar pipeline were determined by ashlized alkali fusion inductively coupled plasma emission spectrometry. Eight elements, such as Al, Si, V, Ni, Fe, Na, Ca and Zn, were detected in the crude oils from the five countries imported from the China-Myanmar pipeline. but P element was not detected in the crude oils. The contents of Fe, V, Si, Ni and other elements are 75.73%, 10.87%, 4.73%, 4.18% and 4.56% respectively.Through analysis, the sino-burmese pipeline crude oil imports of five countries Ni/V and Si/V ratio is less than 1, presents the characteristics of crude oil at sea, oil of different kinds of element contents in there is a difference, and has the certain regularity, between each kind of Ni/V and Si/V ratio were similar, the Fe/V ratio of volatile, can according to the five countries of crude oil for traceability.

Key words: ashing alkali soluble; inductively coupled plasma atomic emission spectrometry; the China-Myanmar pipeline carries crude oil; element

引用本文:李秀林,韩家曦,刘汗青,等.中缅管输进口原油微量元素分析研究[J].化学试剂,2022446908-914.

 

 

利用不稳定Konig体系的中间产物光度法快速测定水中氰化物

李晓惠*,刘海军,许艳广

(辽宁科技学院 药化学院,辽宁 本溪  117004)

 

摘要:以异烟酸、双甲酮分别作为Konig反应的开环、缩合试剂,产生的聚甲炔染料在该异烟酸-双甲酮体系中易分解,该体系为不稳定的Konig体系,但其中间产物具有较高的摩尔吸收系数(ε采用分光光度法获得其中间产物的At曲线,相应建立了快速测定氰化物的新方法。在拟定的实验条件下,该体系的中间产物在531 nm处产生最大吸收ε2.36 × 104 L/(mol·cm),其At曲线呈近似平顶峰形,氰化物浓度在0.0100.800 mg/L范围内与At曲线中的Amax呈良好的线性关系(R = 0.9998,单个样品的测试时间小于5 min方法用于焦化废水中氰化物的测定,回收率在97.9%101.1%之间,RSD1.5%,其测定值与标准方法的测定值吻合,该研究为将Konig反应拓展应用至不稳定体系提供技术参考。

关键词:不稳定Konig体系;双甲酮;中间产物;分光光度法;氰化物;测定

中图分类号:O657.32; X832          文献标识码:A          文章编号0258-32832022

 

Rapid Determination of Cyanide in Water by Spectrophotometry with Intermediate Product of Unstable Konig System LI Xiao-hui*, LIU Hai-jun, XU Yan-guang (Department of Biomedical and Chemical Engineering, Liaoning Institute of Science and Technology, Benxi 117004, China), Huaxue Shiji, 2022, 44(6)

Abstract: In this study, isonicotinic acid and dimedone were used as the ring-opening reagent and condensation reagent of the Konig reaction, respectively. The in situ produced polymethine dye was easily decomposed in the isonicotinic acid-dimedone system which can be determined as an unstable Konig system. However, the intermediate product had a higher molar absorption coefficient (ε), the A~t curve of the intermediate product was obtained by using a new method based on spectrophotometry for the rapid determination of cyanide. In the given experimental condition, the intermediate product of the system has a maximum absorption at 531 nm, featuring an ε of 2.36 × 104 L·mol-1·cm-1. The A~t curve is approximately flat-top peak shaped, the cyanide concentration is in a good linear relationship with the Amax of A~t curve (R = 0.9998) within the range of 0.010 ~ 0.800 mg/L, the testing time of a single sample is less than 5 min. The recovery of our method was between 97.9% ~ 101.1% and the RSD was less than 1.5% when applied to determine the cyanide in coking wastewater, the measured values were in good agreement with that of the standard method. Our study provides technical references for extending the application of the Konig reaction to unstable systems.

Key wordsunstable Konig system; dimedone; intermediate product; spectrophotometry; cyanide; determination

引用本文:李晓惠, 刘海军, 许艳广. 利用不稳定Konig体系的中间产物光度法快速测定水中氰化物[J].化学试剂, 2022, 44(6)915-919.

 

 

【标准物质与标准品】

土壤基质中不同目标浓度重金属标准样品的研制

陈晋,徐冬梅,唐晓菲,张敏*

(安徽省生态环境监测中心,安徽 合肥 230071

 

摘要:介绍了一种土壤重金属标准样品的研制过程。土壤样品经匀浆、干燥、研磨、混匀分瓶包装后,用X射线荧光光谱法对土壤标准样品进行了均匀性、稳定性检验,同时对制备的标准样品进行了定值和不确定度评估。试验结果表明:土壤标准样品均匀性良好,各元素和氧化物的瓶间均匀性不确定度ubb范围为0.02 mg/kg0.043%;在常温避光保存条件下,该土壤标准样品在为期12个月的稳定性检验过程中无不稳定变化趋势;再处理过程对土壤的性质几乎没有影响。该方法是一种简单、有效的制备目标浓度、特定污染因子土壤重金属标准样品的方法。

关键词:X射线荧光光谱法;重金属;土壤;标准样品;目标浓度

中图分类号:X833      文献标识码:A      文章编号0258-32832022--

 

Development of Reference Materials for Heavy Metals in Soil Matrix CHEN Jin, XU Dong-mei, TANG Xiao-fei, ZHANG Min*(Anhui Eco-Environment Monitoring Center, Hefei 230071, China), Huaxue Shiji, 2022, 44(6),

AbstractThe method for the preparation of two heavy metals standard materials with different targeting concentrations in soils matrix has been developed. The samples were prepared by a compound process, including the steps of mixing, drying, grounding, and packing; followed by, homogeneity testing and stability testing were conducted. The value of the standard materials was determined by ICP-OES, ICP-MS, and AFS. The soil standard materials exhibited good homogeneity and stability. Additionally, the uncertainty of the uniformity between bottles (ubb) was 0.02 mg/kg~0.043%, indicating very good uniformity. The standard materials can be stably stored at room temperature for over 12 months without detectable unstable tendency. The reprocessing process exhibited negligible influence on the properties of the standard soil materials. Our method paves a reliable foundation for the development of standard soil materials for simulating heavy metals in the soil matrix.

Key wordsX-ray fluorescence spectrometry; heavy metals; soil; reference materials

引用本文:陈晋,徐冬梅,唐晓菲,等. 土壤基质中不同目标浓度重金属标准样品的研制[J]. 化学试剂,2022446):920-925.

 

 

【合成与工艺技术】

2-1,3-二氢异苯并呋喃)-1-苯乙酮类衍生物的合成

赵美玲1,2, 刘芊芊2, 张翠兰2, 龙思会*1, 李立*2, 刘娥2

(1.武汉工程大学 化工与制药学院,湖北 武汉 4302052.荆楚理工学院 化工与药学院,湖北 荆门 448000

 

摘要:在钴催化体系下,以邻苯二甲醇和苯乙酮为起始原料,一锅法反应得到2-(1,3-二氢异苯并呋喃)-1-苯乙酮,进而对底物进行拓展,得到标题化合物,并对反应条件进行优化。结果表明,以甲苯为溶剂、叔丁醇钾为碱,钴催化剂用量为10%mol,标题化合物的产率较好。化合物结构经1HNMR13CNMR确证。该方法具有反应条件温和、操作简单、产率较高的特点。

关键词:钴催化;邻苯二甲醇;一锅法;2-(1,3-二氢异苯并呋喃)-1-苯乙酮;合成

中图分类号O625.1      文献标识码:A      文章编号:0258-32832022

 

Synthesis of 2-(1,3-Dihydroisobenzofuran)-1-acetophenone Derivatives ZHAO Mei-ling1,2, LIU Qian-qian2, ZHANG Cui-lan2, LONG Si-hui*1, LI Li*2, LIU E2 (1.Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan, 430205, China; 2. College of Chemical Engineering and PharmacyJingchu University of TechnologyJingmen 448000,China), Huaxue shiji, 2022, 44(6)

Abstract: 2-(1,3-dihydroisobenzofuran)-1-acetophenone was synthesized by one pot reaction of phthaloyl alcohol and acetophenone in cobalt catalyzed system. Then, 2-(1,3-dihydroisobenzofuran)- 1-acetophenone derivatives were obtained by expanding the substrates. The reaction conditions were optimized. The results showed that 2- (1,3-dihydroisobenzofuran) -1-acetophenone derivatives (3a3g) were obtained in good yield by using toluene as solvent, potassium tert butyl alcohol as base and 10% mol cobalt as catalyst. The structures of the compounds were confirmed by 1HNMR and 13CNMR. The method is characterized by mild reaction conditions, simple operation and high yield.

Key words: cobalt catalysis; phthaloyl alcoholone pot2-(1,3-dihydroisobenzofuran)-1-acetophenone; synthesis

引用本文赵美玲, 刘芊芊, 张翠兰,等. 2-1,3-二氢异苯并呋喃)-1-苯乙酮类衍生物的合成[J]. 化学试剂,202244(6):926-930

 

 

吴茱萸次碱合成工艺改进

陈仕云1,高永好4,吴宗好4,桂双英2, 3,何勇* 4, 5

1. 合肥学院 分析测试中心,安徽 合肥  2306012. 药物制剂技术与应用安徽省重点实验室,安徽 合肥  2300123. 安徽中医药大学 药学院,安徽 合肥  2300124. 合肥华方医药科技有限公司,安徽 合肥  2300885. 合肥工业大学 化学与化工学院,安徽 合肥  230009)

 

摘要:以靛红、色胺为起始原料,缩合得到N-(2-氨基苯甲酰基)色胺,在硫酸氢钠存在下与原甲酸三乙酯经Pictet-Spengler反应合成了7,8,13b,14-四氢吲哚并[2',3':3,4]吡啶并[2,1-b]喹唑啉-5(7H)-酮,最后芳构化制备吴茱萸次碱,总产率55.8%。目标化合物结构经1HNMR13CNMRESI-MS确证。该工艺反应条件温和、操作简单、原料易得、成本低廉、适用于工业化生产。

关键词:吴茱萸次碱;环合;Pictet-Spengler反应;合成;改进

中图分类号:R914.5      文献标识码:A       文章编号:0258-32832022--

 

Improved Synthesis of Rutaecarpine CHEN Shi-yun1, GAO Yong-hao4, WU Zong-hao4, GUI Shuang-ying2,3, HE Yong*4,5 (1. Analytical & Testing Center, Hefei University, Hefei 230601, China; 2. Anhui Province Key Laboratory of Pharmaceutical Preparation Technology and Application, Hefei 230012, China; 3. Department of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China; 4. Hefei Huafang Pharmaceutical Technology Co., Ltd., Hefei 230088, China; 5. School of chemistry and chemical engineering, Hefei University of technology, Hefei 230009, China), Huaxue Shiji, 2022, 44(6),

Abstract: N-(2-aminobenzoyl) tryptamine was firstly prepared using Indigo and tryptamine as the starting materials by condensation reaction. Then, 7, 8, 13b, 14-tetrahydroindolo [2',3':3,4] pyrido [2,1-b] quinazoline-5(7H)-one was synthesized using triethyl orthoformate in the presence of sodium bisulfate following the Pictet Spengler reaction. Finally, the rutaecarpine was prepared by aromatization with a total yield of 55.8%. The target compound has been confirmed by using 1HNMR13CNMR and ESI-MS. Our improved processes have the merits of mild reaction conditions, simple operation, easy availability of raw materials, and low costs, which are suitable for industrial production.

Key words: rutaecarpine; cyclization; pictet-spengler reaction; synthesis; improvement

引用本文:陈仕云,高永好,吴宗好,等. 吴茱萸次碱合成工艺改进[J]. 化学试剂,2022, 44(6)931-935.

 

 

硫酸苯肼的合成及分析方法

祁锴铌1, 2,辜顺林1, 2,刘建武1, 2,张 2,严生虎* 1, 2

(1.常州大学 药学院,江苏 常州  2131642.石油和化工行业连续流技术工程实验室,江苏 常州  213164)

 

摘要:以苯胺、硫酸、亚硝酸钠为原料,经过重氮化反应、还原反应、酸化反应合成了硫酸苯肼,探索了最佳合成工艺条件,在进行重氮化反应时,采用了连续流微通道反应器,大大缩短了时间,解决了重氮化反应过程中易飙温失控的问题,极大的保证了人员安全,且降低能耗、节约成本,为硫酸苯肼工业化生产提供了参考。同时采用了HPLC对产品进行分析,峰形尖锐对称,分离效果较好,为生产硫酸苯肼的纯度分析提供一些参考。

关键词:硫酸苯肼;连续流;合成;高效液相色谱法;分析

中图分类号:TQ246.3          文献标识码:A          文章编号:0258-32832022

 

Synthesis and Analysis Method of Phenylhydrazine Sulfate QI Kai-ni1,2, GU Shun-lin1,2, LIU Jian-wu1,2, ZHANG Yue 2, YAN Sheng-hu*1,2 (1. School of Pharmacy, Changzhou University, Changzhou 213164, China; 2. Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry, Changzhou 213164, China), Huaxue Shiji, 2022

Abstract: Phenylhydrazine sulfate was synthesized through diazotization reaction, reduction reaction and acidification using aniline, sulfuric acid, and sodium nitrite as raw materials.  The optimal synthesis conditions were explored. A continuous flow microchannel reactor was introduced for the diazotization reaction, which greatly shortened the time and reduced the risk of thermal runaway caused by the strong exothermic diazotization process, therefore, it ensured the safety of personnel, reduced energy consumption, and saved cost. Our research results provide references for the industrial manufacture of phenylhydrazine sulfate. Besides, HPLC detection method was also established to analyze the product, the peak shape was sharp and symmetrical, indicating good separation effect, which provides reliable references for the purity analysis of phenylhydrazine sulfate.

Key words: phenylhydrazine sulfate; continuous flow; synthesis; HPLC; analysis

引用本文:祁锴铌,辜顺林,刘建武,等. 硫酸苯肼的合成及分析方法[J]. 化学试剂,2022446936-940.

 

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