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《化學試劑》2019年第4期中英文摘要

發布時間: 2019-04-10 14:25:24   試劑信息網

農產品中真菌毒素樣品前處理和檢測方法研究進展

王曉1, 2,王秀嬪*1,2,3,4,5,6,李培武*1,2,3,4,5,6,張奇1,3,5,馬飛1,2,4,張文1,3,5,6

1.中國農業科學院油料作物研究所,湖北 武漢  430062;2.農業部油料作物生物學與遺傳育種重點實驗室,湖北 武漢  430062;3.農業部生物毒素檢測重點實驗室,湖北 武漢  430062;4.農業部油料產品質量安全風險評估實驗室,湖北 武漢  430062;5.農業部油料及制品質量監督檢驗測試中心,湖北 武漢  430062,6.國家農業檢測基準實驗室(生物毒素),湖北 武漢  430062

 

摘要:真菌毒素是由真菌產生廣泛存在于農產品中的有毒次生代謝產物。真菌毒素污染日益加重,世界各國真菌毒素限量要求逐年降低,迫切需要更加靈敏、更加準確的真菌毒素確證性檢測技術。系統綜述了農產品中真菌毒素樣品前處理方法和檢測技術,前處理技術包括:液-液萃取技術、固相萃取技術、QuEChERS前處理技術等;檢測技術包括:高效液相色譜法、液相色譜-質譜聯用法、液相色譜-同位素稀釋質譜法等。并對真菌毒素樣品前處理和檢測方法進行了總結和展望。

關鍵詞:真菌毒素;農產品;檢測方法;前處理技術

中圖分類號:TK91    文獻標識碼:A    文章編號: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 Fei1,2,4,ZHANG 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-高效液相色譜串聯質譜法測定花生中黃曲霉毒素的含量

楊代斌1,2,3,喻理1,2,3,4,5,馬飛1,2,3,4,5*,張文1,2,3,4,張奇1,2,3,4,李培武1,2,3,4,5*

1.中國農業科學院油料作物研究所,湖北 武漢  430062;2.農業農村部油料作物生物學與遺傳育種重點實驗室,湖北 武漢  430062;3.國家農業檢測基準實驗室(生物毒素),湖北 武漢  430062;4.農業農村部油料產品質量安全風險評估實驗室,湖北 武漢  430062;5.農業農村部生物毒素檢測重點實驗室,湖北 武漢  430062

 

摘要:建立了磁固相萃取-高效液相色譜串聯質譜(MSPE-HPLC-MS/MS)測定花生黃曲霉毒素的確證性檢測方法,利用甲醇-水溶液對樣品進行提取,使用磁性固相萃取材料萃取、富集和凈化樣品初提液中的黃曲霉毒素,高效液相色譜串聯質譜定量檢測。對影響磁性固相萃取效率的條件進行了優化,主要包括吸附劑用量、萃取溶劑濃度、萃取時間、洗脫劑選擇、洗脫周期等。結果表明,黃曲霉毒素在其線性范圍內線性關系良好,相關系數均大于0.9982,回收率為91.0%120.2%,相對標準偏差為1.1%5.6%,檢出限為0.010.04 μg/kg。該方法樣品富集凈化操作簡單、準確可靠、檢出限低,能夠滿足花生樣品黃曲霉毒素的檢測。

關鍵詞:氧化石墨烯;黃曲霉毒素;磁固相萃取法;液相色譜串聯質譜法

中圖分類號:      文獻標識碼:A        文章編號: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偶聯黃曲霉毒素單克隆抗體方法優化

及其應用

胡小風1,2,3,4,張奇1,2,3,4,張文1,2,3,4*,李培武1,2,3,4,5*

1.中國農業科學院油料作物研究所,湖北武漢 430062;2.農業農村部油料作物生物學與遺傳育種重點實驗室,湖北武漢 430062;3.國家農業檢測基準實驗室(生物毒素),湖北武漢 430062;4.農業農村部油料產品質量安全風險評估實驗室,湖北武漢 430062;5.農業農村部生物毒素檢測重點實驗室,湖北武漢 430062

 

摘要:對Crystarose 4B偶聯黃曲霉毒素單克隆抗體的方法進行優化,制備了黃曲霉毒素B1,B2,G1,G2免疫親和柱。采用甲醇-水為提取溶劑,用均質機將樣品的粉碎和毒素提取一步完成,免疫親和柱對提取液進行凈化、富集,收集洗脫液,在UPLC-MS/MS多反應監測(MRM)模式下進行了定性和定量分析。實驗結果表明,該偶聯方法穩定,親和柱回收率在94.4%107.1%之間,相對標準偏差為1.5%4.9%,重復性、再現性和穩定性良好,柱容量可滿足國標檢測要求。采用所建立的方法檢測花生、玉米和小麥實際樣品中的黃曲霉毒素,檢出率分別為15%、10%10%。

關鍵詞Crystarose 4B;黃曲霉毒素;親和柱;液質聯用

中圖分類號:          文獻標識碼:A   文章編號: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 4B;aflatoxin;immunoaffinity column;UPLC-MS/MS

 

黃曲霉毒素飼料基體標準物質研究

趙天天1, 2,張偉1, 2,王秀嬪*1, 2, 3, 4, 5, 6,李培武*1, 2, 3, 4, 5, 6,張奇1, 3, 5, 6,馬飛1, 2, 4,張文1, 3, 5,6

1.中國農業科學院油料作物研究所,湖北 武漢  430062;2.農業部油料作物生物學與遺傳育種重點實驗室,湖北 武漢  430062;3.農業部生物毒素檢測重點實驗室,湖北 武漢  430062;4.農業部油料產品質量安全風險評估實驗室,湖北 武漢  430062;5.農業部油料及制品質量監督檢驗測試中心,湖北 武漢  430062,6.國家農業檢測基準實驗室(生物毒素),湖北 武漢  430062

 

摘要:建立了含黃曲霉毒素B1、B2、G1、G2的飼料基體標準樣品制備、定值和不確定度評估方法。飼料樣品經加標、干燥、輻照滅菌、混勻、分裝、密封制備而得。經過均勻性檢驗、穩定性檢驗、實驗室聯合定值以及不確定度評估等過程,最終確定飼料中黃曲霉毒素B1、B2、G1、G2的量值分別為(71.23±1.60μg/kg、(75.53±1.28μg/kg、(74.87±1.79μg/kg、(75.77±2.68μg/kg。結果表明,飼料基體標準物質的均勻性良好,穩定性符合標準物質技術要求,同時分析并評估了該基體標準物質研制過程中引入的不確定度。該樣品可用于飼料樣品中黃曲霉毒素B1、B2、G1、G2的定性和定量檢測。

關鍵詞:基體標準物質;黃曲霉毒素;聯合定值;不確定度

中圖分類號:O657.7    文獻標識碼:A    文章編號: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, 4,ZHANG 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優化單寧酸絡合鎂的制備條件及抑菌性能

解彩玲,史澤毅,衛鈺茹,劉 明,趙越,楊冬花,靳利娥*

(太原理工大學 化學化工學院,山西 太原  030024)

 

摘要:探討以單寧酸(TA)為原料與氯化鎂在堿性的條件下進行絡合反應制備單寧酸絡合鎂(T-Mg)的最佳合成條件,并研究了T-Mg的抑菌性能。在單因素實驗的基礎上,采用響應曲面法(RSM)對T-Mg制備條件進行優化,通過傅里葉紅外光譜、紫外光譜、X-射線衍射表征其結構。響應面優化實驗表明,物料比、反應溫度、反應pHT-Mg產率均有顯著影響,優化得到的T-Mg最佳制備條件為n(單寧酸): n(氯化鎂)=1 : 2.70、反應溫度為44 ℃,pH8.0,在該條件下T-Mg產率可達81.91%。以大腸桿菌和金黃色葡萄球菌為供試菌,采用濾紙片法觀察了T-Mg對供試菌的抑菌性能。結果表明,T-Mg對供試菌均有抑制作用,抑菌活性依次為金黃色葡萄球菌、大腸桿菌。T-Mg對供試菌的抑菌效果強于TA,并且隨著T-Mg質量濃度的增加,抑菌效果增強。

關鍵詞:單寧酸;單寧酸絡合鎂;響應曲面法;抑菌性能

中圖分類號:O629    文獻標識碼:A        文章編號: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

 

 

雙靶點抗組胺化合物的設計、合成及活性研究

吳清晨1,許勤龍2,莫佳佳2,趙炎2,朱啟華3,何廣衛2,儲昭興*2,李家明*1

(1.安徽中醫藥大學,安徽 合肥  230031;2.合肥醫工醫藥有限公司,安徽 合肥  230088;3.中國藥科大學 藥物化學教研室,江蘇 南京  210009)

 

摘要:H1受體拮抗劑地氯雷他定為基本骨架,采用藥效團和生物電子等排體原理,設計合成了3個新型具有H1/H4雙重拮抗活性的化合物,并對其進行了體外H1/H4靶點活性檢測、LPS致小鼠急性炎癥因子釋放和組胺誘導小鼠皮膚血管通透性實驗研究。實驗結果顯示,3個化合物均具有H1/H4雙重拮抗活性和顯著的抗炎、抗過敏活性,且可減少LPS誘導小鼠TNF-α釋放(P<0.01),抑制組胺引起的毛細血管通透性增高(P<0.01),抗炎、抗過敏活性優于地氯雷他定和盧帕他定,具有很高的開發價值。

關鍵詞:組胺;抗炎;抗過敏;同源建模;分子對接

中圖分類號:R914.2          文獻標識碼:A            文章編號: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-丁酸類衍生物的合成及體外降糖活性研究

張吉泉*a ,b,杜瑤a,王興蘭a,文林靜a,馬曉a,湯磊b

(貴州醫科大學 a. 藥學院,b. 化學合成藥物研發利用工程技術研究中心,貴州 貴陽  550004

 

摘要:以4-芐氧基苯肼鹽酸鹽及4-氧代庚酸乙酯為原料,經Fischer吲哚環合、還原、酰胺化及水解等步驟得到7個吲哚-3-丁酸衍生物。吲哚-3-丁酸衍生物的結構均經高分辨質譜、核磁共振氫譜及碳譜確證。采用人肝癌HepG2細胞來評價所合成目標化合物的體外降糖活性。結果表明,吲哚-3-丁酸衍生物均具有一定的降糖活性。其中,4-(5-芐氧基-1-(4-甲磺?;郊柞;?/span>)-2-甲基-2,3-二氫-吲哚-3-)丁酸的降糖活性強于陽性對照二甲雙胍,但略微弱于先導化合物GY3。為后續衍生物的設計與合成提供了新思路。

關鍵詞:吲哚,降糖活性,腺苷酸活化蛋白激酶,合成

中圖分類號R914     文獻標識碼A     文章編號: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進展

甘宜遠a, b,田坤c,漆亞云a, b,胡偉男a, b,陳潔a, b,李文a, b,孟嬌a, b,王貞超*a, b,歐陽貴平*a, b, c

(貴州大學 a.藥學院,b. 貴州省合成藥物工程實驗室,c. 精細化工研究開發中心,貴州 貴陽  550025

 

摘要:吲哚酮結構是很多藥物的重要活性基團,含這類結構的化合物通常具有消炎、殺菌、抗病毒、抗高血壓和抗腫瘤等生物活性。吲哚酮類化合物因具有廣譜的生物活性和潛在的藥效研究價值,是藥物研究的熱點。按照結構分類,分別就亞胺類、硫脲類、酰腙類、亞甲基類以及聯氨類3-取代吲哚酮衍生物,及其在抑菌和抗腫瘤等方面的生物活性進行概述,以期為該類化合物的藥物化學方面的研究提供參考價值。

關鍵詞3-取代吲哚酮;生物活性;研究進展

中圖分類號:R9      文獻標識碼:A      文章編號: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

 

淺述香豆素類化合物的抗菌活性

彭莘媚*,潘旭玲,聞軒,王鐵闖,趙云峰,賀銀菊,曹茂啟,王江河

(黔南民族師范學院 化學化工學院,貴州 都勻  558000

 

摘要:香豆素類化合物因其天然資源優勢、結構簡單、易于合成、活性多樣、用途廣泛等特點受到研究者的廣泛關注。特別是香豆素類化合物具有的優良抗耐藥菌活性,再次掀起香豆素抗菌活性的研發熱情?;诮陙硐愣顾仡惢衔锟咕钚缘难芯扛艣r,初步總結了香豆素類化合物在醫藥和農藥兩方面的抗菌研究進展,并對此類化合物的后續研究和發展趨勢進行了簡要展望。

關鍵詞:香豆素;抗細菌;抗真菌;醫藥;農藥

中圖分類號:O622.5           文獻標識碼:A           文章編號: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介孔沸石負載CHCA用于MALDI-TOF-MS分析恩諾沙星小分子化合物的初探

李鵬,楊夢瑞,王敏*,劉芳,周劍,張麗媛

(中國農業科學院 農業質量標準與檢測技術研究所 農產品質量與食物安全重點開放實驗室,北京  100081

 

摘要:本研究考察了Beta沸石材料負載傳統有機基質α-氰基-4-羥基肉桂酸(CHCA),應用于基質輔助激光解吸電離-飛行時間質譜(MALDI-TOF-MS)分析恩諾沙星藥物小分子的效果。實驗中,分別制備了質子、鈉離子及銀離子交換的Beta沸石,并在相同質譜條件下進行了比較研究,考察了不同離子交換的Beta沸石以及CHCA/Beta Na不同混合比例對恩諾沙星藥物小分子的檢測效果。實驗結果表明,使用不同離子交換的Beta沸石作為基質材料,能夠實現恩諾沙星藥物小分子的選擇性離子化,同時,Beta Na沸石負載CHCA新型復合基質用于恩諾沙星藥物小分子的分析中,具有較理想的抑制干擾碎片離子、提高恩諾沙星質譜峰強度等效果。此外,結合前期研究認為,沸石表面活性位點與恩諾沙星藥物小分子存在相互作用關系,進而影響MALDI-TOF-MS質譜分析的離子化效率。

關鍵詞:Beta沸石;激光解吸電離-飛行時間質譜;小分子化合物;恩諾沙星

中圖分類號: O657.63    文獻標識碼: A    文章編號: 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.

 

氟蟲腈及其代謝物氟蟲腈砜中主要有機雜質的定性及定量

鄧超1,張偉*2,李明2,全燦2,張輝1,黃挺2,何雅娟2,李紅梅2

(1.浙江省計量科學研究院,浙江 杭州  310018;2.中國計量科學研究院 化學計量與分析科學研究所,北京  100029)

 

摘要:建立了一種氟蟲腈及其代謝物氟蟲腈砜標準物質侯選物中的主要有機雜質定性、定量分析的方法。采用高效液相色譜-三重四極桿串聯質譜法(HPLC-MS/MS)成功鑒別出氟蟲腈中雜質分別為氟蟲腈砜和氟蟲腈硫化物,而氟蟲腈砜中雜質為氟蟲腈硫化物,推導出其氟蟲腈砜的結構式。HPLC-MS/MS外標法測定氟蟲腈中雜質氟蟲腈砜和氟蟲腈硫化物的含量分別為0.18%、0.47%,相對標準偏差分別為0.73%、0.87%;氟蟲腈砜中雜質氟蟲腈硫化物的含量為0.25%,相對標準偏差為8.05%。該方法的研究對食品安全檢驗中氟蟲腈及氟蟲腈砜的準確測定具有重要意義。

關鍵詞:氟蟲腈;氟蟲腈砜;有機雜質;液相色譜-三重四極桿串聯質譜法;定性;定量

中圖分類號:O657.63    文獻標識碼:A    文章編號: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

 

近紅外光譜法快速篩查減肥類保健品中的咖啡因

彭夢俠*,姚婉清,陳梓云,余永剛

(嘉應學院 化學與環境學院,廣東 梅州  514015

 

摘要:用近紅外光譜法建立了一種減肥類保健品中咖啡因的快速篩查方法。以15種市售減肥類保健品為研究對象,采用甲醇萃取,采集萃取液的近紅外透射光譜圖,利用TQ Analyst 9.0 軟件,采用化學計量學的判別分析法建立了減肥類保健品中咖啡因的快速篩查模型。用此模型檢測了10種市售減肥類保健品,結果表明,含咖啡因的陽性樣品、陰性樣品識別正確率都為100%,誤判數為0。

關鍵詞:近紅外光譜;判別分析法;快速篩查;咖啡因;減肥類保健品

中圖分類號O657.33    文獻標識碼:A    文章編號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

 

 

超高效液相色譜-串聯質譜法測定豆芽中21

植物生長調節劑

黃志波1,何健安1,梁志剛1,何少斌1,李艷芳*2

1.東莞市農產品質量安全監督檢測所,廣東 東莞  523086,2.東莞市農業科學研究中心,廣東 東莞  523086

 

摘要:建立了超高效液相色譜-質譜/質譜法(UPLC-MS/MS)測定豆芽中多種植物生長調節劑殘留量的方法。樣品用酸化乙腈提取,濃縮置換試劑,經0.22 μm濾膜過濾,以C18色譜柱分離待測物,采用多反應監測(MRM)離子掃描模式,外標法進行定量,線性良好,相關系數均大于0.990。21種植物生長調節劑的方法檢出限為0.0010.005 mg/kg,樣品添加回收率為61.5%118.3%,相對標準偏差為0.6%8.3%n=6)。該方法簡單快捷,定量準確,可滿足豆芽中21種植物生長調節劑的殘留檢測要求。

關鍵詞:超高效液相色譜-質譜/質譜法;植物生長調節劑;殘留量;豆芽

中圖分類號:O6   文獻標識碼:A    文章編號:0258-32832019

 

Determination of 21 Plant Growth Regulator in Bean Sprouts by UPLC-MS/MS HUANG Zhi-bo1,HE Jian-an1, LIANG Zhi-gang1, HE Shao-bin1, LI Yan-fang*2 (1. DongGuan Supervision And Test Institution Of Agricultural Produts Quality And Safety,Dongguan 523086, China; 2. Agriculture Research Center of Dongguan,Dongguan 523086,China), 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 mm,1.7 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

 

 

氣相色譜內標法測定白酒中甲醇的不確定度評定

姚怡*,張浩明

(江蘇省無錫市錫山區疾病預防控制中心,江蘇 無錫  214101)

 

摘要:利用氣相色譜內標法對白酒中的甲醇含量進行測定,對測量結果進行不確定度評定。依據JJF 1059.1—2012《測量不確定度評定與表示》建立數學模型,分析實驗過程中各不確定度來源,計算各不確定度分量,進而評定氣相色譜內標法測定白酒中甲醇的不確定度。經檢測白酒中甲醇含量為89.7 mg/L,計算得其擴展不確定度為13.5 mg/L(包含因子k = 2)。結果表明標準曲線的線性回歸是影響該方法不確定度產生的主要因素。在測定時應加強這方面的控制,從而提高測量結果的準確性。

關鍵詞: 不確定度;甲醇;氣相色譜;內標法

中圖分類號:O657.7   文獻標識碼:A     文章編號: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

 

光譜法研究胞磷膽堿鈉與牛血清白蛋白的相互作用

韓永光1,2,壽先苗1,李曉飛*1,2

1. 河南中醫藥大學 藥學院,河南 鄭州 450006;

2. 呼吸疾病診療與新藥研發河南省協同創新中心,河南 鄭州 450046

 

摘要采用紫外-可見分光光度法、熒光光譜法、圓二色譜法(CD)等方法研究胞磷膽堿鈉(CTS)與牛血清白蛋白(BSA)的相互作用。隨著胞磷膽堿鈉濃度的增加,BSA最大吸收峰發生了紅移,蛋白質親水性增加。同步熒光結果也表明,色氨酸和酪氨酸周圍的微環境不斷從疏水性趨向于親水。胞磷膽堿鈉導致 BSA產生靜態熒光猝滅,通過計算得到在溫度298 K時,兩者的結合數約為1,結合常數為8.14×105。胞磷膽堿鈉與BSA相互作用是一個放熱過程(△H <0),也是一個熵增過程(△S >0),其作用力類型主要為靜電作用力。CD結果表明,胞磷膽堿鈉導致BSA 的二級結構發生改變,使其 α-螺旋結構含量增加,β-折疊和無規則卷曲均減少。

關鍵詞:胞磷膽堿鈉;牛血清白蛋白;紫外-可見光譜;熒光光譜;圓二色譜

中圖分類號:O657.3           文獻標識碼:A          文章編號:0258-32832019

 

Spectroscopic Analysis of Interaction between Citicoline Sodium and Bovine Serum Albumin HAN Yong-guang1,2,SHOU 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 sodium;bovine serum albumin;ultraviolet-visible spectrum;fluorescence spectroscopy;circular dichroism spectroscopy

 

 

三氯卡班純度標準物質的定值及不確定度分析

王家睿1,2,陳黎明1,李杰1,吳建軍1,李春華1,陳鷹1,李永利*1

1.上海市計量測試技術研究院,上海  201203;2.東北育才雙語學校高中部,遼寧 沈陽  110164

 

摘要:建立了三氯卡班純度標準物質的定值分析、不確定度評定和制備方法。采用兩種不同原理的測試方法(質量平衡法和定量核磁共振法)對三氯卡班進行了純度定值研究;運用液相色譜法對三氯卡班的分裝樣品進行均勻性檢驗和穩定性考察(包括短期運輸條件穩定性和長期儲存條件穩定性);并評定了不確定度。統計結果表明三氯卡班純度標準物質在95%的置信區間具有良好的均勻性和穩定性。三氯卡班純度標準物質定值結果的標準值和相對擴展不確定度分別為99.3%0.5%k = 2)。本研究對于檢驗檢測工作中三氯卡班的準確測量及量值溯源具有重要意義。

關鍵詞:三氯卡班;標準物質;質量平衡法;定量核磁法

中圖分類號:TQ421.3    文獻標識碼:A    文章編號: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 Ying,LI 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

 

 

固體超強酸固定床催化裂解松香的研究

李修剛,丁謙,吳宜佩,李選維,張玲鈺*

(銅仁學院 材料與化學工程學院,貴州 銅仁  554300)

摘要為了擴展松香的應用范圍,SO42-/MxOy型固體超強酸為催化劑,采用固定床工藝對松香進行深度裂解制備農藥溶劑,研究了固定床工藝條件對松香裂解效果的影響。實驗結果表明,當m(乙二醇二甲醚): m(松香) = 2 : 1,反應溫度為320 ?C、進料速度為0.9 mL/min時,松香裂解效果最佳,酸值為0.87 mg KOH/g,密度0.962 g/mL,裂解油收率達到82.4%,所得產品符合重芳烴農藥溶劑的基本要求。

關鍵詞:固定床;松香;固體超強酸;催化裂解;農藥溶劑

中圖分類號:TQ252.3    文獻標識碼:A      文章編號: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

 

超臨界CO2萃取漢麻3種大麻酚工藝及其抑菌性研究

張旭,孫宇峰,崔寶玉*,高寶昌,田媛,石雨

(黑龍江省科學院大慶分院,黑龍江 大慶  163319)

 

摘要:建立了超臨界CO2萃取漢麻3種大麻酚工藝,考察了其萃取物抑菌效能。通過相應單因素與正交試驗分析,確定了超臨界CO2萃取漢麻3種大麻酚的最佳工藝:萃取溫度45 ℃、萃取時間70 min、夾帶劑用量300 mL、萃取次數3次。對大腸桿菌與金黃色葡萄球菌MIC分別為8 mg/mL6 mg/mL條件下進行濾紙片法抑菌試驗。此條件下大麻二酚(CBD)為3.189 mg/g,六氫大麻酚(CBN)為2.206 mg/g,四氫大麻酚(THC)為58.757 mg/g,即3種大麻酚為64.152 mg/g。大腸桿菌與金黃色葡萄球菌抑菌圈直徑分別為15.4 mm25.8 mm,此超臨界萃取物具有一定的抑菌性能。

關鍵詞:超臨界CO2萃??;漢麻;大麻酚;萃取工藝;抑菌性 

中圖分類號:S563.3             文獻標識碼:A             文章編號: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 way,CBD 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 mm,The supercritical extract has antibacterial effect.

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

 

通過Gabriel反應合成經典化學發光試劑魯米諾

張勝海1, 2, 3,夏忠麗3,郭衛松3,鄒茜茜3,李佳佳3,王長偉3,章成波3,李吉哲3,李曦豪3,

呂家根*1

1. 陜西師范大學 化學化工學院 陜西省生命分析重點實驗室,陜西 西安  710062;2.安康學院 化學化工學院,陜西 安康  725000;3.陜西省漢陰中學,陜西 安康  725100

 

摘要: 3-硝基鄰苯二甲酸為起始原料,先通過一鍋煮的方法,連續實現酐交換、開環和閉環三步反應而得到關鍵中間體N-甲基-3-硝基鄰苯二甲酰亞胺。在40%水合肼溶液中,該中間產物在100 ℃條件下發生Gabriel反應生成環酰肼,同時,中間體苯環上的硝基在自制催化劑FeOOH作用下被水合肼還原為氨基。兩個反應同步完成,極大的縮短了生產周期、反應溫度較低、合成方法及操作簡單、成本低、收率高、污染小,適用于工業化生產。在優化條件下,以83.4 %的總產率得到了超過現有技術標準的魯米諾。

關鍵詞: 合成;化學發光;試劑;魯米諾

中圖分類號:O621.3        文獻標識碼:A          文章編號: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, China;2. School of Chemistry and Chemical Engineering, An'kang University, An'kang 725000, China;3. 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

 

 

對甲苯磺酸控制的β-咔啉衍生物微波輔助合成

付玉軒1,胡珊珊2,郭利杰3,李小娟*1

(新疆師范大學 化學化工學院, 新疆 烏魯木齊  830054

 

摘要:采用對甲苯磺酸(TsOH)作為添加劑,在微波反應器中使色氨酸與醛類5 min內完全轉化為相應的1-取代-四氫-β-咔啉。實驗表明:在色氨酸與脂肪族醛或芳香族醛發生反應的過程中,質子酸作為添加劑起到了關鍵性作用。當該反應采用TsOH作為添加劑時,脂肪族醛與色氨酸反應得到了較好的結果,反應生成的1-取代-四氫-β-咔啉衍生物產率高達95%。1-取代-四氫-β-咔啉衍生物作為合成β-咔啉衍生物的關鍵中間體,其可在MnO2或酸性K2Cr2O7的氧化作用下合成β-咔啉衍生物。

關鍵詞:四氫-β-咔啉;β-咔啉衍生物;微波輔助合成

中圖分類號:0626       文獻標識碼:A       文章編號: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

 


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