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《化学试剂》2019年第4期中英文摘要

农产品中真菌毒素样品前处理和检测方法研究进展

王晓1, 2,王秀嫔*1,2,3,4,5,6,李培武*1,2,3,4,5,6,张奇1,3,5,马飞1,2,4,张文1,3,5,6

1.中国农业科学院油料作物研究所,湖北 武汉  4300622.农业部油料作物生物学与遗传育种重点实验室,湖北 武汉  4300623.农业部生物毒素检测重点实验室,湖北 武汉  4300624.农业部油料产品质量安全风险评估实验室,湖北 武汉  4300625.农业部油料及制品质量监督检验测试中心,湖北 武汉  4300626.国家农业检测基准实验室(生物毒素),湖北 武汉  430062

 

摘要:真菌毒素是由真菌产生广泛存在于农产品中的有毒次生代谢产物。真菌毒素污染日益加重,世界各国真菌毒素限量要求逐年降低,迫切需要更加灵敏、更加准确的真菌毒素确证性检测技术。系统综述了农产品中真菌毒素样品前处理方法和检测技术,前处理技术包括:液-液萃取技术、固相萃取技术、QuEChERS前处理技术等;检测技术包括:高效液相色谱法、液相色谱-质谱联用法、液相色谱-同位素稀释质谱法等。并对真菌毒素样品前处理和检测方法进行了总结和展望。

关键词:真菌毒素;农产品;检测方法;前处理技术

中图分类号:TK91    文献标识码:A    文章编号:0258-32832019

 

Progress of Sample Preparation and Detection of Mycotoxin in Agricultural Products WANG Xiao1,2, WANG Xiu-pin*1,2,3,4,5,6, LI Pei-wu*1,2, 3,4,5,6, ZHANG Qi1,3,5, MA Fei1,2,4ZHANG Wen1,3,5,6 (1.Oil Crops Research Institute, Chinese Academy of Agricultural Sciences, Wuhan 430062, China; 2. Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture, Wuhan 430062, China; 3. Key laboratory of Detection for Mycotoxins, Ministry of Agriculture, Wuhan 430062, China; 4. Laboratory of Risk Assessment for Oilseeds Products(Wuhan), Ministry of Agriculture, Wuhan 430062, China; 5.Quality Inspection and Test Center for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China; 6. National Reference Laboratory for Agricultural Testing P. R. China, Wuhan 430062, China), Huaxue Shiji, 2019, 41(4)

Abstract: Mycotoxins are toxic metabolites that produced by the fungus and are widely exists in agricultural products. Mycotoxin pollution is becoming increasingly serious, and the limit of mycotoxin in various countries is decreasing year by year. There is an urgent need for more sensitive and accurate assay techniques for mycotoxin. This paper systematically reviews the methods for sample preparation and detection of mycotoxins in agricultural products. The preparation techniques include: liquid-liquid extraction, solid phase extraction, QuEChERS preparation technique, and so on; Detection techniques include: high performance liquid chromatography, liquid chromatography-isotope dilution mass spectrometry, liquid chromatography-mass spectrometry and the like. Finally, the sample preparation and detection methods for mycotoxin were summarized and prospected.

Key words: Mycotoxins; agricultural products; detection; pretreatment techniques

 

磁性氧化石墨烯固相萃取-高效液相色谱串联质谱法测定花生中黄曲霉毒素的含量

杨代斌1,2,3,喻理1,2,3,4,5,马飞1,2,3,4,5*,张文1,2,3,4,张奇1,2,3,4,李培武1,2,3,4,5*

1.中国农业科学院油料作物研究所,湖北 武汉  4300622.农业农村部油料作物生物学与遗传育种重点实验室,湖北 武汉  4300623.国家农业检测基准实验室(生物毒素),湖北 武汉  4300624.农业农村部油料产品质量安全风险评估实验室,湖北 武汉  4300625.农业农村部生物毒素检测重点实验室,湖北 武汉  430062

 

摘要:建立了磁固相萃取-高效液相色谱串联质谱(MSPE-HPLC-MS/MS)测定花生黄曲霉毒素的确证性检测方法,利用甲醇-水溶液对样品进行提取,使用磁性固相萃取材料萃取、富集和净化样品初提液中的黄曲霉毒素,高效液相色谱串联质谱定量检测。对影响磁性固相萃取效率的条件进行了优化,主要包括吸附剂用量、萃取溶剂浓度、萃取时间、洗脱剂选择、洗脱周期等。结果表明,黄曲霉毒素在其线性范围内线性关系良好,相关系数均大于0.9982,回收率为91.0%120.2%,相对标准偏差为1.1%5.6%,检出限为0.010.04 μg/kg。该方法样品富集净化操作简单、准确可靠、检出限低,能够满足花生样品黄曲霉毒素的检测。

关键词:氧化石墨烯;黄曲霉毒素;磁固相萃取法;液相色谱串联质谱法

中图分类号:      文献标识码:A        文章编号:0258-32832019

 

Determination of Aflatoxins in Peanut by High Performance Liquid Chromatography-triple Quadrupole Mass Spectrometry with Magnetic Graphene Oxide Solid Phase Extraction Material YANG Dai-bin1,2,3, YU Li1,2,3,4,5, MA Fei1,2,3,4,5*, ZHANG Wen1,2,3,4, ZHANG Qi1,2,3,4, LI Pei-wu1,2,3,4,5* (1.Oil Crops Research Institute of the Chinese Academy of Agricultural Sciences, Wuhan 430062, China; 2.Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China; 3.National Standard Laboratory for Agricultural Testing (Mycotoxins), Wuhan 430062, China; 4.Laboratory of Risk Assessment for Oilseeds Products, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China; 5.Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China),Huaxue Shiji, 2019, 41(4),~

 

Abstract: A method for the determination of aflatoxins in peanuts by magnetic solid phase extraction-high performance liquid chromatography-triple quadrupole mass spectrometry (MSPE-HPLC-MS/MS) was developed. Firstly, peanut sample was extracted with methanol-water, and then the extraction solvent was enriched and purified by magnetic solid phase extraction materials. Aflatoxins were analyzed by HPLC-MS/MS. Several parameters, which could affect the extraction efficiency including materials amount, methanol concentration, extraction time, eluent solvent selection, eluent and elution cycle, were optimized accordingly. Under the optimized conditions, the linear relationships were good and the correlation coefficients were greater than 0.9982. The recovery of aflatoxins ranging from 91.0%120.2%, and the relative standard deviations between 1.1%5.6%, the limit of detection were 0.010.04 μg/kg. This method was simple, accurate and reliable for the detection and purification with good detection limit, which could be applied to the routine analyze of aflatoxins in peanuts.

Key words: graphene oxide; aflatoxins; magnetic solid-phase extraction; HPLC-MS/MS

 

 

Crystarose 4B偶联黄曲霉毒素单克隆抗体方法优化

及其应用

胡小风1,2,3,4,张奇1,2,3,4,张文1,2,3,4*,李培武1,2,3,4,5*

1.中国农业科学院油料作物研究所,湖北武汉 4300622.农业农村部油料作物生物学与遗传育种重点实验室,湖北武汉 4300623.国家农业检测基准实验室(生物毒素),湖北武汉 4300624.农业农村部油料产品质量安全风险评估实验室,湖北武汉 4300625.农业农村部生物毒素检测重点实验室,湖北武汉 430062

 

摘要:对Crystarose 4B偶联黄曲霉毒素单克隆抗体的方法进行优化,制备了黄曲霉毒素B1B2G1G2免疫亲和柱。采用甲醇-水为提取溶剂,用均质机将样品的粉碎和毒素提取一步完成,免疫亲和柱对提取液进行净化、富集,收集洗脱液,在UPLC-MS/MS多反应监测(MRM)模式下进行了定性和定量分析。实验结果表明,该偶联方法稳定,亲和柱回收率在94.4%107.1%之间,相对标准偏差为1.5%4.9%,重复性、再现性和稳定性良好,柱容量可满足国标检测要求。采用所建立的方法检测花生、玉米和小麦实际样品中的黄曲霉毒素,检出率分别为15%10%10%

关键词Crystarose 4B;黄曲霉毒素;亲和柱;液质联用

中图分类号:          文献标识码:A   文章编号:0258-3283(2019)

 

Optimization of Crystarose 4B Coupling Aflatoxin Monoclonal Antibody and Its Application HU Xiao-feng, ZHANG Qi, ZHANG Wen*, LI Pei-wu* (1.Oil Crops Research Institute of the Chinese Academy of Agricultural Sciences, Wuhan 430062, China; 2.Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China; 3.National Standard Laboratory for Agricultural Testing (Mycotoxins), Wuhan 430062, China; 4.Laboratory of Risk Assessment for Oilseeds Products, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China; 5.Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China), Huaxue Shiji, 2019, 41(4), ~

AbstractThe method of coupling Crystarose 4B to aflatoxin monoclonal antibody was optimized, and aflatoxin B1, B2, G1, G2 immunoaffinity column was prepared. Sample preparation was simplified and utilized with a methanol-water solution in a one-step grinding extraction step. The extract was then purified using the home-made immunoaffinity column followed by UPLC-MS/MS for quantification. The results showed that the coupling method was stable, the recoveries ranged from 94.4% to 107.1%, with the relative standard deviations (RSDs) of 1.5%4.9%. The immunoaffinity column demonstrated considerable repeatability, reproducibility, and stability, and the column capacity can meet the requirements of the national standard. Then the method was applied in the detection of peanut, corn and wheat, with detection rates of 15%, 10% and 10%, respectively.

Key wordsCrystarose 4Baflatoxinimmunoaffinity columnUPLC-MS/MS

 

黄曲霉毒素饲料基体标准物质研究

赵天天1, 2,张伟1, 2,王秀嫔*1, 2, 3, 4, 5, 6,李培武*1, 2, 3, 4, 5, 6,张奇1, 3, 5, 6,马飞1, 2, 4,张文1, 3, 5,6

1.中国农业科学院油料作物研究所,湖北 武汉  4300622.农业部油料作物生物学与遗传育种重点实验室,湖北 武汉  4300623.农业部生物毒素检测重点实验室,湖北 武汉  4300624.农业部油料产品质量安全风险评估实验室,湖北 武汉  4300625.农业部油料及制品质量监督检验测试中心,湖北 武汉  4300626.国家农业检测基准实验室(生物毒素),湖北 武汉  430062

 

摘要:建立了含黄曲霉毒素B1B2G1G2的饲料基体标准样品制备、定值和不确定度评估方法。饲料样品经加标、干燥、辐照灭菌、混匀、分装、密封制备而得。经过均匀性检验、稳定性检验、实验室联合定值以及不确定度评估等过程,最终确定饲料中黄曲霉毒素B1B2G1G2的量值分别为(71.23±1.60μg/kg、(75.53±1.28μg/kg、(74.87±1.79μg/kg、(75.77±2.68μg/kg。结果表明,饲料基体标准物质的均匀性良好,稳定性符合标准物质技术要求,同时分析并评估了该基体标准物质研制过程中引入的不确定度。该样品可用于饲料样品中黄曲霉毒素B1B2G1G2的定性和定量检测。

关键词:基体标准物质;黄曲霉毒素;联合定值;不确定度

中图分类号:O657.7    文献标识码:A    文章编号:0258-32832019

 

Study on Matrix Reference Material for Aflatoxins in Feed ZHAO Tian-tian1, 2, ZHANG Wei1, 2, WANG Xiu-pin*1, 2, 3, 4, 5, 6, LI Pei-wu*1, 2, 3, 4, 5, 6, ZHANG Qi1, 3, 5, 6, MA Fei1, 2, 4ZHANG Wen1, 3, 5, 6 (1.Oil Crops Research Institute, Chinese Academy of Agricultural Sciences, Wuhan 430062, China; 2.Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture, Wuhan 430062, China; 3.Key laboratory of Detection for Mycotoxins, Ministry of Agriculture, Wuhan 430062, China; 4.Laboratory of Risk Assessment for Oilseeds Products(Wuhan), Ministry of Agriculture, Wuhan 430062, China; 5.Quality Inspection and Test Center for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China; 6.National Reference Laboratory for Agricultural Testing P. R. China, Wuhan 430062, China), Huaxue, Shiji, 2019, 41(4)

AbstractA method for preparation, certification and uncertainty assessment of feed matrix reference material with aflatoxin B1, aflatoxin B2, aflatoxin G1 and aflatoxin G2 was established. Feed samples were prepared by adding standard, drying, irradiation sterilization, mixing, packing and sealing. With homogenization test, stability test, laboratory joint determination and uncertainty evaluation, the amounts of aflatoxin B1, B2, G1 and G2 in the feed were determined, values were (71.23±1.60), (75.53±1.28), (74.87±1.79), (75.77±2.68) μg/kg. Uniformity of the feed matrix reference material was well, and its stability met the technical requirements of standard materials. Uncertainty caused by development process of the matrix reference material was also measured. The matrix reference material could be used for qualitative and quantitative detection of aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2 in feed samples.

Key words: matrix reference material; aflatoxin; laboratory joint determination; uncertainty

 

RSM优化单宁酸络合镁的制备条件及抑菌性能

解彩玲,史泽毅,卫钰茹,刘 明,赵越,杨冬花,靳利娥*

(太原理工大学 化学化工学院,山西 太原  030024)

 

摘要:探讨以单宁酸(TA)为原料与氯化镁在碱性的条件下进行络合反应制备单宁酸络合镁(T-Mg)的最佳合成条件,并研究了T-Mg的抑菌性能。在单因素实验的基础上,采用响应曲面法(RSM)对T-Mg制备条件进行优化,通过傅里叶红外光谱、紫外光谱、X-射线衍射表征其结构。响应面优化实验表明,物料比、反应温度、反应pHT-Mg产率均有显著影响,优化得到的T-Mg最佳制备条件为n(单宁酸): n(氯化镁)=1 : 2.70、反应温度为44 ℃,pH8.0,在该条件下T-Mg产率可达81.91%。以大肠杆菌和金黄色葡萄球菌为供试菌,采用滤纸片法观察了T-Mg对供试菌的抑菌性能。结果表明,T-Mg对供试菌均有抑制作用,抑菌活性依次为金黄色葡萄球菌、大肠杆菌。T-Mg对供试菌的抑菌效果强于TA,并且随着T-Mg质量浓度的增加,抑菌效果增强。

关键词:单宁酸;单宁酸络合镁;响应曲面法;抑菌性能

中图分类号:O629    文献标识码:A        文章编号:0258-3283(2019)

 

Optimization of Preparation Conditions and Antibacterial Activities of Tannic Acid Complexing Magnesium by RSM XIE Cai-ling, SHI Ze-yi, WEI Yu-ru, LIU Ming, ZHAO Yue, YANG Dong-hua, JIN Li-e* (College of Engineering and Technology, Taiyuan University of Technology, Taiyuan 030024, China), Huaxue Shiji, 2019, 41(4),

Abstract: The aim of this work was to optimize synthesis conditions and investigate antibacterial activities of tannic acid complexing magnesium. Tannic acid complexing magnesium was synthesized from tannic acid and magnesium chloride as raw materials under alkaline conditions. On the basis of single factor test, response surface methodology was applied to optimize the main synthesis conditions. The structure and properties were characterized by FT-IR, UV and XRD. The result showed that the optimum synthesis conditions of optimized tannic acid complexing magnesium were n (tannic acid): n (magnesium chloride) = 1 : 2.70, reaction temperature 44 , and pH 8.0. Under these optimized conditions, the yield of tannic acid complexing magnesium was 81.91%.

The antibacterial properties of tannic acid complexing magnesium against Escherichia coli and staphylococcus aureus were observed by the filter paper method. The results showed that tannic acid complexing magnesium had inhibitory effects on these tested strains, and the antimicrobial activities were Staphylococcus aureus > Escherichia coli. Tannic acid complexing magnesium had generally stronger antibacterial activities on these tested strains than that of tannic acid, and the antibacterial activities were enhanced with the increase of the mass concentration of tannic acid complexing magnesium.

Key words: tannic acid; tannic acid complexing magnesium; response surface methodology; antibacterial activity

 

 

双靶点抗组胺化合物的设计、合成及活性研究

吴清晨1,许勤龙2,莫佳佳2,赵炎2,朱启华3,何广卫2,储昭兴*2,李家明*1

(1.安徽中医药大学,安徽 合肥  2300312.合肥医工医药有限公司,安徽 合肥  2300883.中国药科大学 药物化学教研室,江苏 南京  210009)

 

摘要:H1受体拮抗剂地氯雷他定为基本骨架,采用药效团和生物电子等排体原理,设计合成了3个新型具有H1/H4双重拮抗活性的化合物,并对其进行了体外H1/H4靶点活性检测、LPS致小鼠急性炎症因子释放和组胺诱导小鼠皮肤血管通透性实验研究。实验结果显示,3个化合物均具有H1/H4双重拮抗活性和显著的抗炎、抗过敏活性,且可减少LPS诱导小鼠TNF-α释放(P<0.01),抑制组胺引起的毛细血管通透性增高(P<0.01),抗炎、抗过敏活性优于地氯雷他定和卢帕他定,具有很高的开发价值。

关键词:组胺;抗炎;抗过敏;同源建模;分子对接

中图分类号:R914.2          文献标识码:A            文章编号:0258-3283(2019)

 

Design, Synthesis and Activity of Double Target Antihistamine Compounds WU Qing-chen1, XU Qin-long2, MO Jia-jia2, ZHAO Yan2, ZHU Qi-hua3, HE Guang-wei2, CHU Zhao-xing2*, LI Jia-ming1* (1.Anhui University of Chinese Medicine, Hefei 230031, China; 2.Hefei Medical Engineering Pharmaceutical Co., Ltd., Hefei 230088, China; 3.Department of Medicinal Chemistry, China Pharmaceutical University, Nanjing 210009, China), Huaxue Shiji, 2019, 41(4),

Abstract: Objective: To design and synthesize novel compounds with H1/H4 dual antagonistic activity, and evaluate their bioactivities. Method: H1 Receptor antagonist desloratadine as the basic framework, three novel compounds were designed and synthesized by pharmacophore and bioisosterism strategies. Then the three novel compounds were evaluated for H1/H4 target activity in vitro, also for anti-inflammatory and anti-allergic activity by establishing LPS induced acute inflammatory model and histamine-induced skin capillary permeability model in mice. Results: Compounds 1c, 2c, and 3c showed H1/H4 dual antagonistic activity, reduced the level of LPS-induced TNF-α release in mice(P<0.01), and suppressed the increase of histamine-induced capillary permeability (P<0.01), which showed that compounds 1c, 2c and 3c had anti-inflammatory and anti-allergic activity. Conclusion: Three novel structure compounds have been synthesized and shown to have H1/H4 dual antagonistic activity, and significant anti-inflammatory and anti-allergic activity ,which have high development value.

Key words: histamine; anti-inflammatory; anti-allergy; homology modeling; molecular docking

 

吲哚-3-丁酸类衍生物的合成及体外降糖活性研究

张吉泉*a ,b,杜瑶a,王兴兰a,文林静a,马晓a,汤磊b

(贵州医科大学 a. 药学院,b. 化学合成药物研发利用工程技术研究中心,贵州 贵阳  550004

 

摘要:以4-苄氧基苯肼盐酸盐及4-氧代庚酸乙酯为原料,经Fischer吲哚环合、还原、酰胺化及水解等步骤得到7个吲哚-3-丁酸衍生物。吲哚-3-丁酸衍生物的结构均经高分辨质谱、核磁共振氢谱及碳谱确证。采用人肝癌HepG2细胞来评价所合成目标化合物的体外降糖活性。结果表明,吲哚-3-丁酸衍生物均具有一定的降糖活性。其中,4-(5-苄氧基-1-(4-甲磺酰基苯甲酰基)-2-甲基-2,3-二氢-吲哚-3-)丁酸的降糖活性强于阳性对照二甲双胍,但略微弱于先导化合物GY3。为后续衍生物的设计与合成提供了新思路。

关键词:吲哚,降糖活性,腺苷酸活化蛋白激酶,合成

中图分类号R914     文献标识码A     文章编号:0258-3283(2019)--

 

Synthesis and in Vitro Hypoglycemic Activity of Indole-3-butyric Acid Derivatives ZHANG Ji-quan*a, b, DU Yaoa, WANG Xing-lana, WEN Lin-jinga, MA Xiaoa, Tang Leib1. College of Pharmacy, 2. Engineering Technology Research Center for Chemical Drug R&D, Guizhou Medical University, Guiyang 550004, ChinaHuaxue Shiji, 2019, 41(4),

Abstract: Starting from ethyl 6-oxoheptanoate and (4-(benzyloxy)phenyl)hydrazine hydrochloride, 7 indole-3-butyric acid derivatives were synthesized. All the target compounds were confirmed by high resolution mass spectrometer (HR-MS) and nuclear magnetic resonance (NMR) H and C spectrum. The in vitro hypoglycemic assay in HepG2 cell lines showed that all the target compounds exhibited certain glucose consumption activity. Among of which, compound 1d showed the most potent hypoglycemic activity, but it was less potent than lead compound GY3 yet, which was provided reference for further structural modification.

Key words: indole; hypoglycemic activity; AMP-activated protein kinase; synthesis

 

3-取代吲哚酮衍生物的生物活性研究进展

甘宜远a, b,田坤c,漆亚云a, b,胡伟男a, b,陈洁a, b,李文a, b,孟娇a, b,王贞超*a, b,欧阳贵平*a, b, c

(贵州大学 a.药学院,b. 贵州省合成药物工程实验室,c. 精细化工研究开发中心,贵州 贵阳  550025

 

摘要:吲哚酮结构是很多药物的重要活性基团,含这类结构的化合物通常具有消炎、杀菌、抗病毒、抗高血压和抗肿瘤等生物活性。吲哚酮类化合物因具有广谱的生物活性和潜在的药效研究价值,是药物研究的热点。按照结构分类,分别就亚胺类、硫脲类、酰腙类、亚甲基类以及联氨类3-取代吲哚酮衍生物,及其在抑菌和抗肿瘤等方面的生物活性进行概述,以期为该类化合物的药物化学方面的研究提供参考价值。

关键词3-取代吲哚酮;生物活性;研究进展

中图分类号:R9      文献标识码:A      文章编号:0258-3283(2019)

 

Progress of 3-Substitution Indolone Derivatives GAN Yi-yuana, b, TIAN Kunc, QI Ya-yuna, b, HU Wei-nana, b, CHEN Jiea, b, LI Wena, b, MENG Jiaoa, b, WANG Zhen-chao*a,b, OUYANG Gui-ping*a, b, c (a. College of Pharmacy, b. Guizhou Engineering Laboratory for Synthetic Drugs, c. Center for Research and Development of Fine Chemicals, Guizhou University, Guiyang 550025, China), Huaxue Shiji, 2019, 41(4)

AbstractIndolone is an important active group of many drugs, and compounds containing such structure usually have anti-inflammatory, bactericidal, anti-viral, anti-hypertensive, anti-tumor and other biological activities. Herein, indolone compounds have become a hot spot in drug research because of their broad-spectrum biological activity and potential pharmacodynamic research value. In this work, based on the structure, 3-substituted indolone derivatives were divided into imines, thioureas, hydrazides, methylenes and hydrazine, and the biological activity in terms of antibacterial and antitumor were summarized. It is hoped to provide reference value for the research of these compounds on pharmacochemistry.

Key words3-substitution indolone; bioactivity; research progress

 

浅述香豆素类化合物的抗菌活性

彭莘媚*,潘旭玲,闻轩,王铁闯,赵云峰,贺银菊,曹茂启,王江河

(黔南民族师范学院 化学化工学院,贵州 都匀  558000

 

摘要:香豆素类化合物因其天然资源优势、结构简单、易于合成、活性多样、用途广泛等特点受到研究者的广泛关注。特别是香豆素类化合物具有的优良抗耐药菌活性,再次掀起香豆素抗菌活性的研发热情。基于近年来香豆素类化合物抗菌活性的研究概况,初步总结了香豆素类化合物在医药和农药两方面的抗菌研究进展,并对此类化合物的后续研究和发展趋势进行了简要展望。

关键词:香豆素;抗细菌;抗真菌;医药;农药

中图分类号:O622.5           文献标识码:A           文章编号:0258-32832019--

 

Progress in Antibacterial Activity of Coumarins PENG Xin-mei*, PAN Xu-ling, WEN Xuan, WANG Tie-chuang, ZHAO Yun-feng, HE Yin-ju, CAO Mao-qi, WANG Jiang-he (School of Chemistry and Chemical Engineering, Qiannan Normal University for Nationalities, Duyun 558000, China), Huaxue Shiji, 2019, 41(4)   

Abstract: Coumarins have attracted much attention due to the natural resource, simple structure, easy synthesis, diverse activities and wide applications. Especially, coumarins have been found to have excellent activity against resistant bacteria, which has aroused researchers' enthusiasm for the development of antibacterial activity of coumarins. In this work, based on the general situation of coumarins' antibacterial activity in recent years, the progress in antibacterial activity of coumarins in medicine and pesticide was summarized, and the follow-up research and development trend of coumarins were prospected.

Key words: coumarin; antibacterial; antifungal; medicine; pesticide

 

Beta介孔沸石负载CHCA用于MALDI-TOF-MS分析恩诺沙星小分子化合物的初探

李鹏,杨梦瑞,王敏*,刘芳,周剑,张丽媛

(中国农业科学院 农业质量标准与检测技术研究所 农产品质量与食物安全重点开放实验室,北京  100081

 

摘要:本研究考察了Beta沸石材料负载传统有机基质α-氰基-4-羟基肉桂酸(CHCA),应用于基质辅助激光解吸电离-飞行时间质谱(MALDI-TOF-MS)分析恩诺沙星药物小分子的效果。实验中,分别制备了质子、钠离子及银离子交换的Beta沸石,并在相同质谱条件下进行了比较研究,考察了不同离子交换的Beta沸石以及CHCA/Beta Na不同混合比例对恩诺沙星药物小分子的检测效果。实验结果表明,使用不同离子交换的Beta沸石作为基质材料,能够实现恩诺沙星药物小分子的选择性离子化,同时,Beta Na沸石负载CHCA新型复合基质用于恩诺沙星药物小分子的分析中,具有较理想的抑制干扰碎片离子、提高恩诺沙星质谱峰强度等效果。此外,结合前期研究认为,沸石表面活性位点与恩诺沙星药物小分子存在相互作用关系,进而影响MALDI-TOF-MS质谱分析的离子化效率。

关键词:Beta沸石;激光解吸电离-飞行时间质谱;小分子化合物;恩诺沙星

中图分类号: O657.63    文献标识码: A    文章编号: 0258-32832019

 

Analysis of Enrofloxacin by Matrix Assisted Laser Desorption Ionization Time-of-flight Mass Spectrometry with CHCA Loading on Beta Zeolite as Composite Matrix LI Peng, YANG Meng-rui, WANG Min*, LIU Fang, ZHOU Jian, ZHANG Li-yuan (Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agriculture, Beijing 100081, China), Huaxue Shiji, 2019, 41(4),

Abstractα-Cyano-4-hydroxycinnamic acid (CHCA) loading on beta zeolite as novel composite matrix was applied in matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analysis of enrofloxacin. In the experiments, H+, Na+ and Ag+ ion exchanged beta zeolites were prepared, respectively. These new matrixes were examined and compared in the analysis of enrofloxacin at the same MALDI-TOF-MS conditions. The results indicated that the enrofloxacin could be selectively ionized by using metal ion exchanged zeolite. Additionally, CHCA loading on beta Na zeolite with the mass ratio of 4 : 2 was capable of suppressing fragments and promotingpeak intensity of enrofloxacin. Based on previous research, it was presumed that the interaction between the activity site on zeolite surface and enrofloxacin would affect the ionization efficiency of MALDI-TOF-MS analysis.

 

氟虫腈及其代谢物氟虫腈砜中主要有机杂质的定性及定量

邓超1,张伟*2,李明2,全灿2,张辉1,黄挺2,何雅娟2,李红梅2

(1.浙江省计量科学研究院,浙江 杭州  3100182.中国计量科学研究院 化学计量与分析科学研究所,北京  100029)

 

摘要:建立了一种氟虫腈及其代谢物氟虫腈砜标准物质侯选物中的主要有机杂质定性、定量分析的方法。采用高效液相色谱-三重四极杆串联质谱法(HPLC-MS/MS)成功鉴别出氟虫腈中杂质分别为氟虫腈砜和氟虫腈硫化物,而氟虫腈砜中杂质为氟虫腈硫化物,推导出其氟虫腈砜的结构式。HPLC-MS/MS外标法测定氟虫腈中杂质氟虫腈砜和氟虫腈硫化物的含量分别为0.18%0.47%,相对标准偏差分别为0.73%0.87%;氟虫腈砜中杂质氟虫腈硫化物的含量为0.25%,相对标准偏差为8.05%。该方法的研究对食品安全检验中氟虫腈及氟虫腈砜的准确测定具有重要意义。

关键词:氟虫腈;氟虫腈砜;有机杂质;液相色谱-三重四极杆串联质谱法;定性;定量

中图分类号:O657.63    文献标识码:A    文章编号:0258-32832019

 

Analysis of the Organic Impurities in Fipronil and Metabolite Fipronil Sulfone DENG Chao1, ZHANG Wei*2, LI Ming2, QUAN Can2, ZHANG Hui1, HUANG Ting2, HE Ya-juan2, LI Hong-mei21.Zhejiang Province Institute of Metrology, Zhejiang 310018, China; 2.Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China), Huaxue Shiji, 2019, 41(4)

Abstract: Qualitative and quantitative analysis of the major organic impurities in pure fipronil and its metabolite fipronil sulfone in polluted eggs was performed. The organic impurities were qualitatively determined by high performance liquid chromatography-triple quarupole tandem mass spectrometry (HPLC-MS/MS)Full scan of LC/MS in positive ion mode was firstly executed to obtain the m/z values of the molecules. Then LC-MS/MS was

carried out on target compounds to obtain structural information. Impurities 1 and 2 in fipronil were successfully identified as fipronil sulfone and fipronil sulphide, respectively. The molecular structure of impurity 1 was derived and impurity 2 in fipronil sulfone was successfully identified as fipronil sulphide. HPLC-MS/MS external standard method was used to determine the content of the organic impurities. There are 0.18% fipronil sulfone with the RSD of 0.73% and 0.47% fipronil sulphide with the RSD of 0.87% in pure fipronil material. The content of impurity 2 in fipronil sulfone material was 0.25% with the RSD of 8.05%. Moreover, this method has instructive significance to the qualitative and quantitative analysis of pure fipronil and fipronil sulfone and other pure organic substances. The accuracy of determination of fipronil and fipronil sulfone in egg and lay the foundation for development of a national first grade certified reference material of fipronil and fipronil sulfone.

Key words: fipronil; fipronil sulfone ;organic impurities; HPLC-MS/MS; qualitative; quantitative

 

近红外光谱法快速筛查减肥类保健品中的咖啡因

彭梦侠*,姚婉清,陈梓云,余永刚

(嘉应学院 化学与环境学院,广东 梅州  514015

 

摘要:用近红外光谱法建立了一种减肥类保健品中咖啡因的快速筛查方法。以15种市售减肥类保健品为研究对象,采用甲醇萃取,采集萃取液的近红外透射光谱图,利用TQ Analyst 9.0 软件,采用化学计量学的判别分析法建立了减肥类保健品中咖啡因的快速筛查模型。用此模型检测了10种市售减肥类保健品,结果表明,含咖啡因的阳性样品、阴性样品识别正确率都为100%,误判数为0

关键词:近红外光谱;判别分析法;快速筛查;咖啡因;减肥类保健品

中图分类号O657.33    文献标识码:A    文章编号0258-3283(2019)--

 

Rapid Screening of Caffeine in Weight-reducing Health Product by Near-infrared Spectroscopy PENG Meng-xia*, YAO Wan-qing, CHEN Zi-yun, YU Yong-gang (School of Chemistry and Environment, Jiaying University, Meizhou 514015, China) Huaxue Shiji, 2019, 41(4),     

Abstract: The method of rapid screening of caffeine in weight-reducing health product was investigated. Taking 15 kinds of weight-reducing health products as the object, the recognition model of caffeine was established using FT-NIR combined with discriminant analysis. The model was used to detect the 10 samples, and the results showed that the correct recognition rate of model was 100%, and the miscarriage of justice was 0.

Key words: FT-NIR; discriminant analysis; rapid screening; caffeine; weight-reducing health product

 

 

超高效液相色谱-串联质谱法测定豆芽中21

植物生长调节剂

黄志波1,何健安1,梁志刚1,何少斌1,李艳芳*2

1.东莞市农产品质量安全监督检测所,广东 东莞  5230862.东莞市农业科学研究中心,广东 东莞  523086

 

摘要:建立了超高效液相色谱-质谱/质谱法(UPLC-MS/MS)测定豆芽中多种植物生长调节剂残留量的方法。样品用酸化乙腈提取,浓缩置换试剂,经0.22 µm滤膜过滤,以C18色谱柱分离待测物,采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好,相关系数均大于0.99021种植物生长调节剂的方法检出限为0.0010.005 mg/kg,样品添加回收率为61.5%118.3%,相对标准偏差为0.6%8.3%n=6)。该方法简单快捷,定量准确,可满足豆芽中21种植物生长调节剂的残留检测要求。

关键词:超高效液相色谱-质谱/质谱法;植物生长调节剂;残留量;豆芽

中图分类号:O6   文献标识码:A    文章编号:0258-32832019

 

Determination of 21 Plant Growth Regulator in Bean Sprouts by UPLC-MS/MS HUANG Zhi-bo1HE Jian-an1, LIANG Zhi-gang1, HE Shao-bin1, LI Yan-fang*2 (1. DongGuan Supervision And Test Institution Of Agricultural Produts Quality And SafetyDongguan 523086, China; 2. Agriculture Research Center of DongguanDongguan 523086China), Huaxue Shiji, 2019, 41(4)

Abstract An effective method of liquid chromatography-mass spectrometry/mass spectrometry (UPLC-MS /MS) was established to detect the residues of various plant growth regulators in bean sprouts. The samples were initially extracted with acetonitrile and concentrated, which were filtered by 0.22 µm filter membrane afterwards. Then the eluate was separated by gradient elution with methanol- water solution of different ratio on C18100 mm×2.1 mm1.7 µm)column. It was detected under the mode of positive multiple reactions monitoring(MRM). The external standard method was adopted for quantitative analysis, the correlation coefficients was more than 0.990. Finally, the detection limit of 21 kinds of plant growth regulators, for all the samples, ranged from 0.001 to 0.005 mg/kg, the recoveries of samples were 61.5% to 118.3% and the relative standard deviations were in the range of 0.6% to 8.3 %(n = 6). In conclusion, it is a simple and efficient method which can meet the requirements for residue testing of 21 types of plant growth regulators in bean sprouts.

Key wordsUPLC-MS/MS; plant growth regulator;      ; bean sprouts

 

 

气相色谱内标法测定白酒中甲醇的不确定度评定

姚怡*,张浩明

(江苏省无锡市锡山区疾病预防控制中心,江苏 无锡  214101)

 

摘要:利用气相色谱内标法对白酒中的甲醇含量进行测定,对测量结果进行不确定度评定。依据JJF 1059.1—2012《测量不确定度评定与表示》建立数学模型,分析实验过程中各不确定度来源,计算各不确定度分量,进而评定气相色谱内标法测定白酒中甲醇的不确定度。经检测白酒中甲醇含量为89.7 mg/L,计算得其扩展不确定度为13.5 mg/L(包含因子k = 2)。结果表明标准曲线的线性回归是影响该方法不确定度产生的主要因素。在测定时应加强这方面的控制,从而提高测量结果的准确性。

关键词: 不确定度;甲醇;气相色谱;内标法

中图分类号:O657.7   文献标识码:A     文章编号:0258-32832019

 

Evaluation of Uncertainty in Measurement of Methanol in Liquor by Gas Chromatographic Internal Standard Method YAO Yi*, ZHANG Hao-ming (Xishan District of Center for Disease Prevention and Control, Wuxi 214101, China), Huaxue Shiji, 2019, 41(4)

Abstract: The content of methanol in liquor was measured by using gas chromatographic internal standard method. The uncertainty of measurement result was evaluated. Based on JJF 1059.1-2012”Evaluation and Expression of Uncertainty in Measurement”, a mathematic model was established to analyze the sources of uncertainty and calculate the uncertain components during the experiment process. The model was used to assess the uncertainty of the internal standard method to measure the methanol in liquor. The content of methanol in liquor was 89.7 mg/L, and the extended uncertainty was 13.5 mg/L (including factor k=2).The main factor influencing the uncertainty of this method was the linear regression of the standard curve. The control on the standard curve should be reinforced in order to improve the accuracy of determination.

Key words: uncertainty; methanol; gas chromatography; internal standard method

 

光谱法研究胞磷胆碱钠与牛血清白蛋白的相互作用

韩永光1,2,寿先苗1,李晓飞*1,2

1. 河南中医药大学 药学院,河南 郑州 450006

2. 呼吸疾病诊疗与新药研发河南省协同创新中心,河南 郑州 450046

 

摘要采用紫外-可见分光光度法、荧光光谱法、圆二色谱法(CD)等方法研究胞磷胆碱钠(CTS)与牛血清白蛋白(BSA)的相互作用。随着胞磷胆碱钠浓度的增加,BSA最大吸收峰发生了红移,蛋白质亲水性增加。同步荧光结果也表明,色氨酸和酪氨酸周围的微环境不断从疏水性趋向于亲水。胞磷胆碱钠导致 BSA产生静态荧光猝灭,通过计算得到在温度298 K时,两者的结合数约为1,结合常数为8.14×105。胞磷胆碱钠与BSA相互作用是一个放热过程(△H <0),也是一个熵增过程(△S >0),其作用力类型主要为静电作用力。CD结果表明,胞磷胆碱钠导致BSA 的二级结构发生改变,使其 α-螺旋结构含量增加,β-折叠和无规则卷曲均减少。

关键词:胞磷胆碱钠;牛血清白蛋白;紫外-可见光谱;荧光光谱;圆二色谱

中图分类号:O657.3           文献标识码:A          文章编号:0258-32832019

 

Spectroscopic Analysis of Interaction between Citicoline Sodium and Bovine Serum Albumin HAN Yong-guang1,2SHOU Xian-miao1, LI Xiao-fei*1, 21. College of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, China; 2. Collaborative Innovation Center for Respiratory Disease Diagnosis and Treatment and Chinese Medicine Development of Henan Province, Zhengzhou 450046, China), Huaxue Shiji, 2019, 41(4)

AbstractThe interaction between citicoline sodium (CTS) and bovine serum albumin (BSA) was investigated by ultraviolet-visible spectrum, fluorescence quenching and synchronous fluorescence as well as circular dichroism spectra. The protein absorption peak had been found to be redshift and the hydrophilicity raised with the increase of the CTS concentration. Synchronous fluorescence also indicated the protein microenvironment around tryptophan and tyrosine was constantly changing from hydrophobic to hydrophilic. CTS had a strong ability to quench the BSA fluorescence in a static mode. The binding constants was 8.14×105 and the site numbers was close to 1 at 25. The free energy diversificationΔGand entropy changeΔSwere calculated based on Stern-Volmer equation and ΔG<0, ΔS<0, indicating that the main type of force is electrostatic force. The circular dichroism demonstrated that the secondary structure of BSA changed after interacted with CTS, leading to the content of α-helix to increase, accompanied by an decrease in an unordered structure and β-sheet.

Key words: citicoline sodiumbovine serum albuminultraviolet-visible spectrumfluorescence spectroscopycircular dichroism spectroscopy

 

 

三氯卡班纯度标准物质的定值及不确定度分析

王家睿1,2,陈黎明1,李杰1,吴建军1,李春华1,陈鹰1,李永利*1

1.上海市计量测试技术研究院,上海  2012032.东北育才双语学校高中部,辽宁 沈阳  110164

 

摘要:建立了三氯卡班纯度标准物质的定值分析、不确定度评定和制备方法。采用两种不同原理的测试方法(质量平衡法和定量核磁共振法)对三氯卡班进行了纯度定值研究;运用液相色谱法对三氯卡班的分装样品进行均匀性检验和稳定性考察(包括短期运输条件稳定性和长期储存条件稳定性);并评定了不确定度。统计结果表明三氯卡班纯度标准物质在95%的置信区间具有良好的均匀性和稳定性。三氯卡班纯度标准物质定值结果的标准值和相对扩展不确定度分别为99.3%0.5%k = 2)。本研究对于检验检测工作中三氯卡班的准确测量及量值溯源具有重要意义。

关键词:三氯卡班;标准物质;质量平衡法;定量核磁法

中图分类号:TQ421.3    文献标识码:A    文章编号:0258-32832019

 

Purity Determination and Uncertainty Evaluation of Triclocarban Reference Material WANG Jia-rui, CHEN Li-ming, LI Jie, WU Jian-jun, LI Chun-hua, CHEN YingLI Yong-li* (1. Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China; 2.          Shenyang 201203, China), Huaxue Shiji, 2019, 41(4),

AbstractThe method for purity determination, uncertainty evaluation and preparation of triclocarban reference material was establishedThe quantitative analysis was carried out by means of 1HNMR quantitative nuclear magnetic resonance (qNMR) and balance method simultaneously. The homogeneity examination and stability investigation (including short-term transport condition and long-term storage condition) of the triclocarbans ample  was conducted with liquid chromatography method. The trichlorocarban purity reference material had good uniformity and stability in the 95% confidence interval. The certified purity value of the reference material of triclocarban was 99.3% with an relative expanded uncertainty of 0.5% (k=2). It would assure the accuracy of determination of triclocarban.

Key wordstriclocarban; reference material; mass balance method; quantitative nuclear magnetic resonance

 

 

固体超强酸固定床催化裂解松香的研究

李修刚,丁谦,吴宜佩,李选维,张玲钰*

(铜仁学院 材料与化学工程学院,贵州 铜仁  554300)

摘要为了扩展松香的应用范围SO42-/MxOy型固体超强酸为催化剂,采用固定床工艺对松香进行深度裂解制备农药溶剂,研究了固定床工艺条件对松香裂解效果的影响。实验结果表明,当m(乙二醇二甲醚): m(松香) = 2 : 1,反应温度为320 ˚C、进料速度为0.9 mL/min时,松香裂解效果最佳,酸值为0.87 mg KOH/g,密度0.962 g/mL,裂解油收率达到82.4%,所得产品符合重芳烃农药溶剂的基本要求。

关键词:固定床;松香;固体超强酸;催化裂解;农药溶剂

中图分类号:TQ252.3    文献标识码:A      文章编号:0258-32832019--

 

Cracking of Rosin Catalyzed by Solid Superacid in Fixed Bed LI Xiu-gang, DING Qian, WU Yi-pei, LI Xuan-wei, ZHANG Ling-yu* (College of Material and Chemical Engineering, Tongren University,

Tongren 554300, China), Huaxue Shiji, 2019, 41(4)   

Abstract: In the work, rosin was cracked in fixed bed with the catalysis of SO42-/MxOy solid superacid, and a kind of pesticide solvent was obtained. The processing parameters of fixed bed on the production of pyrolysis oil were investigated. The results showed that the optimal mass ratio between solvent and rosin was 2 : 1, the optimal temperature was 320 ˚C, and the feeding rate of reacting material was 0.9 mL/min. The pyrolysis oil was obtained with the acid value 0.87 mg KOH/g, relative density 0.962 g/mL, and the yield of 82.4%, which can reach the standard of heavy aromatic solvent.

Key words: fixed Bed; rosin; solid superacid; catalytic cracking; pesticide solvent

 

超临界CO2萃取汉麻3种大麻酚工艺及其抑菌性研究

张旭,孙宇峰,崔宝玉*,高宝昌,田媛,石雨

(黑龙江省科学院大庆分院,黑龙江 大庆  163319)

 

摘要:建立了超临界CO2萃取汉麻3种大麻酚工艺,考察了其萃取物抑菌效能。通过相应单因素与正交试验分析,确定了超临界CO2萃取汉麻3种大麻酚的最佳工艺:萃取温度45 ℃、萃取时间70 min、夹带剂用量300 mL、萃取次数3次。对大肠杆菌与金黄色葡萄球菌MIC分别为8 mg/mL6 mg/mL条件下进行滤纸片法抑菌试验。此条件下大麻二酚(CBD)为3.189 mg/g,六氢大麻酚(CBN)为2.206 mg/g,四氢大麻酚(THC)为58.757 mg/g,即3种大麻酚为64.152 mg/g。大肠杆菌与金黄色葡萄球菌抑菌圈直径分别为15.4 mm25.8 mm,此超临界萃取物具有一定的抑菌性能。

关键词:超临界CO2萃取;汉麻;大麻酚;萃取工艺;抑菌性 

中图分类号:S563.3             文献标识码:A             文章编号:0258-32832019

 

Extraction Technology and Antibacterial Effect of Three Cannabinoids in Hemp ZHANG Xu, SUN Yu-feng , CUI Bao-yu*, GAO Bao-chang, TIAN Yuan, SHI Yu  (Daqing Branch of Heilongjiang Academy of Sciences, Daqing 163319, China), Huaxue Shiji, 2019, 41(4)

Abstract: To establish a supercritical CO2 extraction method for three cannabinoids in hemp and investigate the antimicrobial activity . The supercritical CO2 extraction method for three cannabinoids in hemp is established based on the analysis of the single factor and orthogonal tests. Three cannabinoids in hemp are extracted at extraction temperature 45 ,extraction time 70 min,entrainment and dosage 300 mL and extraction times for 3.The filter method for bacteriostatic test is established with the MIC of escherichia coli and staphylococcus aureus at 8 mg/mL and 6 mg/mL. By this wayCBD content is 3.189 mg/g, CBN content is 2.206 mg/g, THC content is 58.757 mg/g, so three cannabinoids content is 64.152 mg/g. The bacteriostatic rings of escherichia coli and staphylococcus aureus are 15.4 mmand 25.8 mmThe supercritical extract has antibacterial effect.

Key wordssupercritical CO2 extraction; hemp; cannabinoid; antibacterial activity; extraction process

 

通过Gabriel反应合成经典化学发光试剂鲁米诺

张胜海1, 2, 3夏忠丽3郭卫松3邹茜茜3李佳佳3王长伟3章成波3李吉哲3李曦豪3

吕家根*1

1. 陕西师范大学 化学化工学院 陕西省生命分析重点实验室,陕西 西安  7100622.安康学院 化学化工学院,陕西 安康  7250003.陕西省汉阴中学,陕西 安康  725100

 

摘要: 3-硝基邻苯二甲酸为起始原料,先通过一锅煮的方法,连续实现酐交换、开环和闭环三步反应而得到关键中间体N-甲基-3-硝基邻苯二甲酰亚胺。在40%水合肼溶液中,该中间产物在100 ℃条件下发生Gabriel反应生成环酰肼,同时,中间体苯环上的硝基在自制催化剂FeOOH作用下被水合肼还原为氨基。两个反应同步完成,极大的缩短了生产周期、反应温度较低、合成方法及操作简单、成本低、收率高、污染小,适用于工业化生产。在优化条件下,以83.4 %的总产率得到了超过现有技术标准的鲁米诺。

关键词: 合成;化学发光;试剂;鲁米诺

中图分类号:O621.3        文献标识码:A          文章编号:0258-3283(2019)

 

Synthesis of the Classical Chemiluminescent Reagent Luminol via Gabriel Reaction ZHANG Sheng-hai1,2,3, XIA Zhong-li3, GUO Wei-song3, ZOU Xi-xi3, LI Jia-jia3, WANG Chang-wei3, ZHANG Cheng-bo3, LI Ji-zhe3, LI Xi-hao3, LV Jia-gen*1 (1. Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi'an 710062, China2. School of Chemistry and Chemical Engineering, An'kang University, An'kang 725000, China3. High School of Hanyin County, Shaanxi Province, An'kang 725100, China), Huaxue Shiji, 2019, 41(4)

Abstract: In "one-pot" reaction with three continuously step as anhydride exchange, ring-open and cyclization, the initial material of 3-nitro-phthalic acid was effectively converted to the key intermediate named N-methyl-3-nitro-phthalimide. In 40% hydrazine hydrate solution, ring hydrazide was formed via Gabriel reaction at 100 , meanwhile, the nitro group on the benzene ring was reduced to amino group under the catalysis of home-made FeOOH catalyst. The two-step reactions were completed simultaneously with low reaction temperature, simple method, convenient operation, low cost, high yield and decrease pollution, all of which merits were benefit for the industrial production process. Under the optimization conditions, the total yield of the product reaches up to 83.4 %, higher than the existing technical standard.

Key words: synthesis; chemiluminescence; reagent; luminol

 

 

对甲苯磺酸控制的β-咔啉衍生物微波辅助合成

付玉轩1,胡珊珊2,郭利杰3,李小娟*1

(新疆师范大学 化学化工学院, 新疆 乌鲁木齐  830054

 

摘要:采用对甲苯磺酸(TsOH)作为添加剂,在微波反应器中使色氨酸与醛类5 min内完全转化为相应的1-取代-四氢-β-咔啉。实验表明:在色氨酸与脂肪族醛或芳香族醛发生反应的过程中,质子酸作为添加剂起到了关键性作用。当该反应采用TsOH作为添加剂时,脂肪族醛与色氨酸反应得到了较好的结果,反应生成的1-取代-四氢-β-咔啉衍生物产率高达95%1-取代-四氢-β-咔啉衍生物作为合成β-咔啉衍生物的关键中间体,其可在MnO2或酸性K2Cr2O7的氧化作用下合成β-咔啉衍生物。

关键词:四氢-β-咔啉;β-咔啉衍生物;微波辅助合成

中图分类号:0626       文献标识码:A       文章编号:0258-32832019

 

Microwave Assisted Synthesis of β-carboline Derivatives Controlled by p-Toluenesulfonic Acid FU Yu-xuan1, HU Shan-shan2, GUO Li-jie3, LI Xiao-juan *1 (College of Chemistry and Chemical Engineering, Xinjiang Normal University, Urumqi 830054, China), Huaxue Shiji, 2019, 41(4)

Abstract: p-Toluenesulfonic acid (TsOH) was used as an additive to completely convert tryptophan and aldehydes into corresponding 1-substituted-tetrahydro-β-caroline derivatives in 5 min in a microwave reactor. Experiments show that protonic acid plays a key role in the reaction of tryptophan with aliphatic aldehydes or aromatic aldehydes. When TsOH was used as an additive in the reaction, the reaction of aliphatic aldehydes with tryptophan gives better results. 1-Substituted-tetrahydro-β-caroline derivatives were produced with yields up to 95% by the reaction of aliphatic aldehydes with tryptophan. The 1-substituted-tetrahydro-β-carbaline was employed as the key intermediate for the synthesis of β-carbaline , which can be synthesized β-carboline derivatives under the oxidation of MnO2 or acidic K2Cr2O7.

Key words: tetrahydrogen β-carbolines; β-carbolines derivatives; microwave-assisted synthesis