三种砜吡草唑主要代谢物的合成
作者:
李志洋;尹迪;张宇飞;柳红霞;钟玉君;...
期刊:
合成化学 ,2024年32(9):833-839 ISSN:1005-1511
作者机构:
[李志洋] 中南林业科技大学理学院,湖南长沙 410004;[李志洋] 长沙嘉桥生物科技有限公司,湖南长沙 410000;[谢练武; 周昊; 钟玉君; 彭雨晴] 中南林业科技大学;[尹迪; 赵东江; 柳红霞; 张宇飞] 长沙嘉桥生物科技有限公司
关键词:
砜吡草唑;代谢物;合成路径;工艺优化;毒理试验;农药登记
摘要:
为了满足除草剂代谢物毒理试验的需求,本研究设计并优化了砜吡草唑的3个主要代谢物M1、M3和M4的合成路径。通过全新的合成路径,以1-甲基-3-三氟甲基-4-氯甲基-5-二氟甲氧基-1-H-吡唑为起始原料,经过一系列反应步...展开更多 为了满足除草剂代谢物毒理试验的需求,本研究设计并优化了砜吡草唑的3个主要代谢物M1、M3和M4的合成路径。通过全新的合成路径,以1-甲基-3-三氟甲基-4-氯甲基-5-二氟甲氧基-1-H-吡唑为起始原料,经过一系列反应步骤,成功合成了M1和M3。以2-甲基-2-丙烯酸和溴肟为原料,经过一系列反应后成功合成M4。通过核磁共振氢谱、液相质谱和高效液相色谱等方法对代谢物的结构和纯度进行了确定。经过优化合成工艺,M1、M3和M4的产率分别达到了76.9%、82.5%和70.1%。合成的代谢物纯度可达97%以上。本研究首次从合成路线的角度出发,成功设计并制备了这3种砜吡草唑代谢物,为农药登记和农残质检等领域提供了重要的研究基础。收起
语种:
中文
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Threaded 3D microfluidic paper analytical device-based ratiometric fluorescent sensor for background-free and visual detection of organophosphorus pesticides
作者:
Tong, Xia;Cai, Guihan;Xie, Lianwu* ;Wang, Tongtao;Zhu, Yongfeng;...
期刊:
Biosensors and Bioelectronics ,2023年222:114981 ISSN:0956-5663
通讯作者:
Xie, Lianwu;Shi, SY;Guo, Y
作者机构:
[Shi, SY; Shi, Shuyun; Xie, Lianwu; Peng, Yuqing; Tong, Xia] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;[Shi, Shuyun; Wang, Tongtao; Zhu, Yongfeng; Tong, Chaoying; Tong, Xia; Cai, Guihan] Cent South Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.;[Tong, Xia] Shanxi Med Univ, Shanxi Acad Med Sci, Hosp 3, Shanxi Bethune Hosp, Taiyuan 030032, Shanxi, Peoples R China.;[Guo, Ying; Guo, Y] Cent South Univ, Xiangya Hosp, Dept Clin Pharmacol, Hunan Key Lab Pharmacogenet, Changsha 410078, Hunan, Peoples R China.
通讯机构:
[Shi, SY ; Xie, LW; Guo, Y ] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;Cent South Univ, Xiangya Hosp, Dept Clin Pharmacol, Hunan Key Lab Pharmacogenet, Changsha 410078, Hunan, Peoples R China.
关键词:
Background-free analysis;Organophosphorus pesticide;Ratiometric fluorescent system;Threaded 3D microfluidic paper device;Visual detection
摘要:
With the increasing concerns of food safety and environmental protection, it is desirable to develop reliable, effective, and portable sensors for detection of organophosphorus pesticides (OPs). Here, a cascade reaction system integrated with threaded 3D microfluidic paper analytical device (3D μPAD) was firstly developed for background-free and visual detection of OPs in agricultural samples. Butyrylcholinesterase (BChE) hydrolyzed acetylcholine into thiocholine (TCh), which reduced MnO(2) nanosheets into Mn(2+). With addition of OPs, BChE activity was irreversibly inhibited, and the generation of TCh and the reduction of MnO(2) nanosheets were prevented. Then the remaining MnO(2) nanosheets oxidized o-phenylenediamine into 2,3-diaminophenazine with yellow-emission fluorescence, which quenched the fluorescence intensity of red-emission carbon dots (RCDs) via inner-filter effect. Based on above mechanism, a ratiometric fluorescent system was established for OPs detection. Threaded 3D μPAD consisted of 4 layers, which allowed to load and/or add reagents to trigger the cascade reaction system for OPs detection. The fluorescent images presented distinguishable color variations from red to yellow with dichlorvos concentrations ranging from 2.5 to 120μgL(-1), and the limit of detection was 1.0μgL(-1). In the practical samples testing, threaded 3D μPAD can eliminate background influence on fluorescent signal for OPs detection. Threaded 3D μPAD integrated with ratiometric sensing platform has merits of accuracy response, facile operation, and background-free detection, which supplies a new alternative approach for on-site pesticide detection.
语种:
英文
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新型介离子类酰胺化合物的设计、合成及生物活性
作者:
颜宇;吕亮;吴明慧;相君成;庞怀林;...
期刊:
农药 ,2023年62(06):391-395 ISSN:1006-0413
作者机构:
[谢练武] 中南林业科技大学理学院;[吕亮; 相君成; 吴明慧; 刘吉永; 庞怀林] 南通泰禾化工股份有限公司;[颜宇] 中南林业科技大学理学院<&wdkj&>南通泰禾化工股份有限公司
关键词:
合成;介离子;间二酰胺;杀虫活性
摘要:
[目的]为了发现结构新颖的高效杀虫剂。[方法]利用活性亚结构拼接法合成了一系列介离子类酰胺化合物,其结构经过1H NMR和HRMS确证。[结果]合成了15个结构新颖的介离子类酰胺化合物。生物活性测试结果表明:所合成的化合物对刺吸式害虫苜蓿蚜和朱砂叶螨没有生物活性,但部分化合物对咀嚼式口器害虫小菜蛾和黏虫具有一定活性。特别是化合物2a和2g在100 mg/L时对黏虫致死率为100%,且对小菜蛾致死率能达到80%及以上。[结论]合成的介离子类酰胺化合物具有一定的杀虫活性,为进一步研究提供了参考。
语种:
中文
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Digital image colorimetry on smartphone for chemical analysis: A review
作者:
Fan, Yajun;Li, Jiawei;Guo, Yaping;Xie, Lianwu* ;Zhang, Gui*
期刊:
Measurement ,2021年171:108829 ISSN:0263-2241
通讯作者:
Xie, Lianwu;Zhang, Gui
作者机构:
[Fan, Yajun; Zhang, Gui; Li, Jiawei; Xie, Lianwu; Guo, Yaping] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Peoples R China.;[Zhang, Gui] Cent South Univ Forestry & Technol, Key Lab Digital Dongting Lake Basin Hunan Prov, Changsha 410004, Peoples R China.
通讯机构:
[Xie, LW; Zhang, G] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Peoples R China.
关键词:
Cameras;Color;Colorimeters;Image analysis;Lighting;Medical imaging;Metal analysis;mHealth;Optimization;Smartphones;Analytical procedure;Basic procedure;Camera technology;Continuous development;Continuous optimization;Current status;Lighting conditions;Natural compounds;Colorimetry
摘要:
Digital image colorimetry (DIC) on smartphone is regarded as a powerful, fast and low-cost analysis method to measure target analyte with color changes of digital image obtained by the built-in camera. We summarized the basic procedure of DIC, the color spaces (RGB, CMYK, HSB/HSL, CIE XYZ, L*a*b*, and YUV), the principal architectures (tools for capturing image, lighting conditions, and color quantification APPs and DIC APPs), and current status of DIC on smartphone in analysis of metals/heavy metals, herbicides, pesticides, antibiotics, biological and medical indicators, natural compounds, and bacteria/viruses. The advantages and disadvantages of DIC are also revealed. Nowadays, DIC on smartphone must be further refined with controlled geometry and standard lighting sources to become robust and reliable analytical procedures. And it will be improved in the near future with the continuous development of smartphones owing to the rapid development of smartphone's camera technology and the continuous optimization of related software. © 2020 Elsevier Ltd
语种:
英文
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Rapid and comprehensive profiling of α-glucosidase inhibitors in Buddleja Flos by ultrafiltration HPLC–QTOF-MS/MS with diagnostic ions filtering strategy
作者:
Xie, Lianwu* ;Fu, Qiachi;Shi, Shuyun* ;Li, Jiawei;Zhou, Xinji
期刊:
Food Chemistry ,2021年344:128651 ISSN:0308-8146
通讯作者:
Xie, Lianwu;Shi, Shuyun
作者机构:
[Shi, Shuyun; Xie, Lianwu; Shi, SY; Li, Jiawei; Zhou, Xinji] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Peoples R China.;[Shi, Shuyun; Fu, Qiachi] Cent South Univ, Coll Chem & Chem Engn, Changsha 410083, Peoples R China.
通讯机构:
[Xie, LW; Shi, SY] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Peoples R China.
关键词:
Diagnostic ions filtering;Flavonoid;HPLC–QTOF-MS/MS;Phenylethanoid glycoside;Ultrafiltration;α-Glucosidase inhibitor
摘要:
Buddleja Flos is used as yellow rice colorant and a well-known traditional Chinese medicine. But its biochemical profiling is still lack due to complex matrix. Here, ultrafiltration high-performance liquid chromatograph–quadrupole time-of-flight tandem mass spectrometry (HPLC–QTOF-MS/MS) with diagnostic ions filtering strategy was proposed for rapid and comprehensive investigation of its α-glucosidase inhibitors. As a result, 33 bioactive compounds (13 phenylethanoid glycosides and 20 flavonoids) were successfully screened and identified. In addition, α-glucosidase inhibitory activities of twenty-two references were verified. Six flavonoid aglycones (4, 28, and 30–33) showed excellent α-glucosidase inhibitory activities (IC50, from 5.11 ± 0.85 to 32.49 ± 9.76 μg/mL), much higher than that of acarbose (IC50, 195.49 ± 10.05 μg/mL). Five flavonoid-monoglycosides (7, 12, 13, 20, and 22) presented moderate inhibitory activities with IC50 from 160.98 ± 23.19 to 249.37 ± 35.83 μg/mL. Results showcased the high efficiency of proposed strategy in profiling of bioactive compounds from natural products. © 2020 Elsevier Ltd
语种:
英文
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兽用博落回生物碱的分光光度法测定及提取工艺响应面优化
作者:
周欣吉;李嘉伟;申典灵;颜宇;胡晓鹏;...
期刊:
饲料研究 ,2021年44(22):67-72 ISSN:1002-2813
作者机构:
中南林业科技大学理学院,湖南长沙410004;[谢练武; 颜宇; 申典灵; 周欣吉; 胡晓鹏; 李嘉伟] 中南林业科技大学
关键词:
博落回;生物碱;溴甲酚绿;分光光度法;响应面优化
摘要:
试验旨在提高兽用博落回资源利用率,开发兽用博落回生物碱快速检测方法。在单因素试验基础上,运用响应面法对博落回中总生物碱提取工艺进行优化,并建立数学模型验证其可靠性。优化过程中采用分光光度法测定生物碱含量。结果显示,博落回生物碱的溴甲酚绿分光光度法检测的线性范围为0.000 8~0.008 0 g/L。博落回生物碱提取工艺响应面优化的回归方程显著(P<0.000 1),失拟项不显著(P=0.121 6)。总生物碱得率影响因素的强弱次序为:提取温度>盐酸浓度>液料比>提取时间。在液料比15 mL/g、盐酸浓度0.2 mol/L、提取温度75℃、提取时间1.6 h的最优条件下,实际总生物碱平均得率为30.34 mg/g,与理论预测值吻合。研究表明,建立的博落回生物碱含量溴甲酚绿分光光度法测定方法操作简便、灵敏度高,可用于生物碱含量的快速检测。通过响应面法优化的博落回生物碱提取工艺稳定可靠,在最优条件下可实现资源利用最大化。
语种:
中文
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智能手机数字图片比色分析法概述
作者:
范亚军;李嘉伟;郭亚平;谢练武
期刊:
食品安全质量检测学报 ,2020年11(5):1651-1658 ISSN:2095-0381
作者机构:
中南林业科技大学理学院,长沙 410004;[谢练武; 范亚军; 郭亚平; 李嘉伟] 中南林业科技大学
关键词:
比色分析;智能手机;数字图片;颜色模型;图像传感器;食品安全;快速检测
摘要:
为保护环境与食品安全,有毒有害物质的现场快速检测以及分析数据即时反馈显得越发重要。随着智能手机的广泛普及与其应用程序的不断完善,智能手机数字图片比色分析法得到了快速发展。本文简述了智能手机数字图片比色法的基本原理、图片采集设备及其传感器类型、图片颜色模型、图片数字化软件、分析数据处理与网络共享,以及该方法在食品安全、医疗诊断、生物检测等领域的研究与应用,对数字图片比色分析法未来的发展也做出了展望。得益于智能手机软硬件的不断完善,数字图片比色分析法将得到广泛应用。
语种:
中文
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Cetyltrimethyl ammonium mediated enhancement of the red emission of carbon dots and an advanced method for fluorometric determination of iron(III)
作者:
Li, Te;Xie, Lianwu;Long, Ruiqing;Tong, Chaoying;Guo, Ying;...
期刊:
Microchimica Acta ,2019年186(12):791 ISSN:0026-3672
通讯作者:
Shi, Shuyun;Lin, Qinlu
作者机构:
[Shi, Shuyun; Tong, Chaoying; Tong, Xia; Li, Te; Long, Ruiqing] Cent S Univ, Coll Chem & Chem Engn, Key Lab Hunan Prov Water Environm & Agr Prod Safe, Changsha 410083, Hunan, Peoples R China.;[Shi, Shuyun; Shi, SY; Lin, Qinlu; Xie, Lianwu] Cent South Univ Forestry & Technol, Coll Sci, Coll Food Sci & Engn, Changsha 410004, Hunan, Peoples R China.;[Shi, Shuyun; Guo, Ying] Cent S Univ, Xiangya Hosp, Dept Clin Pharmacol, Hunan Key Lab Pharmacogenet, Changsha 410078, Hunan, Peoples R China.
通讯机构:
[Shi, Shuyun; Shi, SY; Lin, QL] C;Cent S Univ, Coll Chem & Chem Engn, Key Lab Hunan Prov Water Environm & Agr Prod Safe, Changsha 410083, Hunan, Peoples R China.;Cent South Univ Forestry & Technol, Coll Sci, Coll Food Sci & Engn, Changsha 410004, Hunan, Peoples R China.;Cent S Univ, Xiangya Hosp, Dept Clin Pharmacol, Hunan Key Lab Pharmacogenet, Changsha 410078, Hunan, Peoples R China.
关键词:
Fluorometric assay;Human plasma;Metal ion;Nanomaterial;Quenching mechanism;Surface functionalization;Surfactant
摘要:
Red-emissive carbon dots (CDs) were synthesized by one-step hydrothermal technique using citric acid (CA), and urea in N,N-dimethylformamide (DMF) solution. The CDs has an average diameter of 2.3 nm, excitation/emission maxima at 553/606 nm, and a low photoluminescence quantum yield (4%). Fluorescence is weakly quenched by the ions Fe(3+), Hg(2+), Cu(2+), Co(2+), Zn(2+), Ca(2+), Ni(2+), and Pb(2+). After addition of cetyltrimethyl ammonium ion (CTAB), electrostatic interaction between negatively charged CDs and CTAB causes the CDs to self-aggregate. The formation of CD/CTAB increases the average particle diameter to around 13 nm and enhances the quantum yield to 24%. The hydrophobic segments of CTAB twined into a network structure can selectively trap Fe(3+) and then interact with surface groups of the CDs to cause quenching. The CD/CTAB nanoprobe enables fluorometric determination of Fe(3+) with a linear response in the 0.10-10 muM concentration range and a 0.03 muM limit of detection. The probe was utilized for determination of Fe(3+) in human serum samples, and satisfactory results were obtained. Graphical abstractSchematic representation of fluorometric analysis of Fe(III) ion by cetyltrimethyl ammonium ion (CTAB) mediated red emission carbon dots (CDs). The hydrophobic segments of CTAB twined into a network structure can selectively trap Fe(III) and then interact with surface groups of the CDs to cause quenching.
语种:
英文
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Vinyl Phosphate-Functionalized, Magnetic, Molecularly-Imprinted Polymeric Microspheres' Enrichment and Carbon Dots' Fluorescence-Detection of Organophosphorus Pesticide Residues
作者:
Wu, Mao;Fan, Yajun;Li, Jiawei;Lu, Danqing;Guo, Yaping;...
期刊:
Polymers ,2019年11(11):1770 ISSN:2073-4360
通讯作者:
Xie, Lianwu;Wu, Yiqiang
作者机构:
[Fan, Yajun; Wu, Mao; Lu, Danqing; Li, Jiawei; Xie, Lianwu; Guo, Yaping] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;[Wu, Yiqiang] Cent South Univ Forestry & Technol, Coll Mat Sci & Technol, Changsha 410004, Hunan, Peoples R China.
通讯机构:
[Xie, Lianwu; Wu, Yiqiang] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;Cent South Univ Forestry & Technol, Coll Mat Sci & Technol, Changsha 410004, Hunan, Peoples R China.
关键词:
fluorescence detection;magnetic molecularly imprinted polymeric microspheres;organophosphorus pesticides;pesticide residues;sensor
摘要:
The rapid detection of organophosphorus pesticide residues in food is crucial to food safety. One type of novel, magnetic, molecularly-imprinted polymeric microsphere (MMIP) was prepared with vinyl phosphate and 1-octadecene as a collection of dual functional monomers, which were screened by Gaussian09W molecular simulation. MMIPs were used to enrich organic phosphorus, which then detected by fluorescence quenching in vinyl phosphate-modified carbon dots ([email protected]) originated from anhydrous citric acid. MMIPs and [email protected] were characterized by TEM, particle size analysis, FT-IR, VSM, XPS, adsorption experiments, and fluorescence spectrophotometry in turn. Through the fitting data from experiment and Gaussian quantum chemical calculations, the molecular recognition properties and the mechanism of fluorescence detection between organophosphorus pesticides and [email protected] were also investigated. The results indicated that the MMIPs could specifically recognize and enrich triazophos with the saturated adsorption capacity 0.226 mmol g-1, the imprinting factor 4.59, and the limit of recognition as low as 0.0006 mmol L-1. Under optimal conditions, the [email protected] sensor has shown an extensive fluorescence property with a LOD of 0.0015 mmol L-1 and the linear range from 0.0035 mmol L-1 to 0.20 mmol L-1 (R2 = 0.9988) at 390 nm. The mechanism of fluorescence detection of organic phosphorus with [email protected] sensor might be attributable to hydrogen bonds formed between heteroatom O, N, S, or P, and the O-H group, which led to fluorescent quenching. Meanwhile, HN-C=O and Si-O groups in [email protected] system might contribute to cause excellent blue photoluminescence. The fluorescence sensor was thorough successfully employed to the detection of triazophos in cucumber samples, illustrating its tremendous value towards food sample analysis in complex matrix. © 2019 by the authors.
语种:
英文
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Rapidly colorimetric detection of caffeine in beverages by silver nanoparticle sensors coupled with magnetic molecularly imprinted polymeric microspheres
作者:
Deng, Huiyun;Wang, Bin;Wu, Mao;Deng, Bin;Xie, Lianwu* ;...
期刊:
INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY ,2019年54(1):202-211 ISSN:0950-5423
通讯作者:
Xie, Lianwu;Guo, Yaping
作者机构:
[Deng, Huiyun; Wu, Mao; Xie, Lianwu; Wang, Bin; Guo, Yaping] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;[Deng, Bin] Xiangnan Univ, Coll Chem Biol & Environm Engn, Chenzhou 423043, Peoples R China.;[Xie, Lianwu] Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
通讯机构:
[Xie, LW; Guo, YP; Xie, Lianwu] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
关键词:
Caffeine;colorimetric analysis;molecularly imprinted polymeric microspheres;silver nanoparticles
摘要:
Excessively intaking caffeine can harm human health, and it is imperative to develop a rapid method to identify caffeine for food safety. The magnetic molecularly imprinted polymeric microspheres (MMIPs) were prepared to pretreat samples before silver nanoparticles (AgNPs) colorimetric detection of caffeine. Using Fe3O4 as supporting core, mesoporous SiO2 as intermediate shell, α-methylacrylic acid as functional monomer and caffeine as template, the prepared MMIPs were characterised by transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometer. Adsorption process followed Langmuir adsorption isotherm with maximum adsorption capacity at 38.8mgg−1 under 298K. The MMIPs extract caffeine from beverages, then the AgNPs colorimetric method rapidly screened and semi-quantified caffeine ≥5mgL−1 by naked eye, and accurately quantified caffeine ranging 0.1–5mgL−1 by UV-vis spectroscopy at 393nm, which were consistent with HPLC analytical results. Thus, this method might be used to rapidly enrich and analyse caffeine in beverages. © 2018 Institute of Food Science and Technology
语种:
英文
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以《无机及分析化学》为例浅议学生创新能力培养
作者:
郭鑫;袁寒梦;罗秋艳;肖滕;王文磊;...
期刊:
广州化工 ,2019年47(19):146-147,150 ISSN:1001-9677
作者机构:
中南林业科技大学理学院,湖南 长沙,410004;中南林业科技大学材料学院,湖南 长沙,410004;[谢练武; 肖滕; 罗秋艳; 袁寒梦; 王文磊; 郭鑫] 中南林业科技大学
关键词:
教学改革;翻转课堂;化学课程;创新能力
摘要:
针对当前高等林业院校化学课程教学方法单一的现状,以学生创新能力培养为导向,利用"翻转课堂"教学法、"问题式"教学法等多元教学法,进行 《无机及分析化学》 课程教学改革,构建"启发式"、"互动式"、"重基础"与"重创新"四位一体课程教学体系.通过招聘单位对应聘者的满意程度、 大大上升的深造比率、 毕业生对学校培养模式的满意程度、 显著提高的学生创新能力等方面,证明 《无机及分析化学》 课程教学改革方案确实可行.
语种:
中文
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基于翻转课堂的《无机及分析化学》教学改革
作者:
郭鑫;袁寒梦;罗秋艳;肖滕;谢练武;...
期刊:
广州化工 ,2019年47(20):144-145,160 ISSN:1001-9677
作者机构:
中南林业科技大学理学院,湖南 长沙,410004;中南林业科技大学材料学院,湖南 长沙,410004;[谢练武; 肖滕; 罗秋艳; 袁寒梦; 王文磊; 郭鑫] 中南林业科技大学
关键词:
翻转课堂;无机及分析化学;教学改革
摘要:
根据 《无机及分析化学》 课程的教学要求与学生的实际情况,以高等林业院校林产化工及相关专业无机及分析化学的教学情况为依据,采用新的教学模式对公共基础课无机及分析化学进行变革与探索.以 《无机及分析化学》 重要知识点"金属指示剂"一章为例,论述 《无机及分析化学》 教学课堂独特的教学模式及其优势,证实了翻转课堂教学模式能够显著提高学生课堂效率和加强学生科研创新和思辨能力.
语种:
中文
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没食子酸磁性表面分子印迹聚合物的制备与选择性识别性能
作者:
邓慧芸;王斌;吴茂;文瑞芝;马强;...
期刊:
应用化学 ,2018年35(5):600-608 ISSN:1000-0518
作者机构:
中南林业科技大学理学院,应用化学研究所, 长沙, 410004;湘南学院化学生物与环境工程学院, 湖南, 郴州, 423043;[邓慧芸; 王斌; 吴茂; 文瑞芝; 马强; 郭亚平; 谢练武] 中南林业科技大学理学院,应用化学研究所, 长沙, 410004;[邓斌] 湘南学院化学生物与环境工程学院, 湖南, 郴州, 423043
关键词:
表面分子印迹;选择性识别;羟基苯甲酸类化合物;吸附;磁性Fe_3O_4
摘要:
羟基苯甲酸类化合物用途广泛,极性较强,在复杂水溶液体系中这些类似物的分离纯化与分析非常困难.本文以磁性Fe_3O_4纳米颗粒为载体,没食子酸(GA)为模板分子,制备了磁性表面分子印迹聚合物(MIP).利用透射电子显微镜、红外光谱、磁强测定等检测手段对MIP进行了结构表征.并对其吸附性能进行研究,比较了该MIP对GA及其它3种结构类似物的吸附性能差异.结果表明,制备的以GA为模板的磁性分子印迹聚合物为核壳球形结构,键合牢固,对GA的吸附动力学符合准二级动力学方程模型,吸附过程属于Langmuir单分子层吸附.该聚合物对GA表现出优异的选择性识别能力,其吸附量(318 K时37.736 mg /g)远远高于结构类似物.该磁性分子印迹聚合物对模板分子不仅具有特异识别能力,而且能够磁控分离,分离效率高,可用于固相萃取.
语种:
中文
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有机磷农药残留分子印迹聚合物研究现状与展望
作者:
吴茂;范亚军;郭亚平;谢练武
期刊:
农药学学报 ,2018年20(6):689-703 ISSN:1008-7303
作者机构:
[吴茂; 范亚军; 郭亚平; 谢练武] 中南林业科技大学理学院, 长沙, 410004
关键词:
有机磷农药;残留;分子印迹聚合物;计算化学;传感器;仿生催化;样品前处理
摘要:
为解决有机磷农药在土壤及水体中的残留污染问题,分子印迹技术在该类农药残留检测中的应用研究已得到迅速发展。文章就有机磷农药分子印迹聚合物(molecularly imprinted polymers,MIPs)的研究背景、分子印迹技术基本原理及分类、计算化学在筛选优化虚拟模板及功能单体中的应用,以及有机磷农药残留MIPs的制备与应用研究等内容进行了综述。 MIPs因具有结构可预测、特异识别和应用普遍的特性,可广泛用于光学传感、化学传感、电化学传感、光电传感、质量敏感传感、仿生催化及样品前处理等众多领域。可通过Discovery Studio、HyperChem及Gaussian 3种分子模拟软件对(虚拟)模板、功能单体以及二者所形成的加合物进行计算模拟以获得最低能量的优势构象,通过计算加合物的结合能来优化筛选(虚拟)模板和功能单体。将计算化学与实验研究相结合,相信在未来几年,有机磷农药残留MIPs有可能在原位显色传感、农产品农药残留高通量筛查及计算机自动化检测等领域得到长足发展。
语种:
中文
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Magnetic surface molecularly imprinted polymeric microspheres using gallic acid as a segment template for excellent recognition of ester catechins
作者:
Wang, Bin;Deng, Huiyun;Wu, Mao;Xiang, Shu;Ma, Qiang;...
期刊:
ANALYTICAL METHODS ,2018年10(27):3317-3324 ISSN:1759-9660
通讯作者:
Xie, Lianwu;Guo, Yaping
作者机构:
[Ma, Qiang; Shi, Shuyun; Deng, Huiyun; Wu, Mao; Xiang, Shu; Xie, Lianwu; Wang, Bin; Guo, Yaping] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;[Shi, Shuyun; Xie, Lianwu] Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
通讯机构:
[Xie, LW; Guo, YP; Xie, Lianwu] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
摘要:
Magnetic surface molecularly imprinted polymeric microspheres (MMIPs) were prepared by using gallic acid (GA) as a segment template for the solid extraction of ester catechins as a whole from complex samples. MMIPs were characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, and vibrating sample magnetometry. The results of the adsorption experiments indicated that the saturated adsorption capacity of GA on MMIPs was 0.21 mmol g-1, and the imprinting factor was 5.86; MMIPs had higher adsorption capacity for ester catechins than benzoic acid, salicylic acid, and 2,4-dihydroxybenzoic acid. The adsorption process of MMIPs could be better described by pseudo secondary rate equation, and it was consistent with the Langmuir adsorption model. In addition to GA, MMIPs could selectively recognize ester catechins in a tea solution without column packing. Thus, MMIPs prepared using GA as a segment template can be used in selective separation and enrichment of ester catechins from tea samples for functional food production. © 2018 The Royal Society of Chemistry.
语种:
英文
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Rapid colorimetric detection of cartap residues by AgNP sensor with magnetic molecularly imprinted microspheres as recognition elements
作者:
Wu, Mao;Deng, Huiyun;Fan, Yajun;Hu, Yunchu;Guo, Yaping;...
期刊:
Molecules ,2018年23(6):1443 ISSN:1420-3049
通讯作者:
Xie, Lianwu
作者机构:
[Fan, Yajun; Hu, Yunchu; Deng, Huiyun; Wu, Mao; Xie, Lianwu; Guo, Yaping] Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;[Xie, Lianwu] Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
通讯机构:
[Xie, Lianwu] C;Cent South Univ Forestry & Technol, Coll Sci, Changsha 410004, Hunan, Peoples R China.;Cent S Univ, Coll Chem & Chem Engn, Changsha 410083, Hunan, Peoples R China.
关键词:
carbamothioic acid, S,S'-(2-(dimethylamino)-1,3-propanediyl) ester;magnetite;metal nanoparticle;microsphere;silicon dioxide;silver;thiocarbamic acid derivative;chemical structure;chemistry;colorimetry;molecular imprinting;procedures;tea;Colorimetry;Ferrosoferric Oxide;Metal Nanoparticles;Microspheres;Molecular Imprinting;Molecular Structure;Silicon Dioxide;Silver;Tea;Thiocarbamates
摘要:
The overuse of cartap in tea tree leads to hazardous residues threatening human health. A colorimetric determination was established to detect cartap residues in tea beverages by silver nanoparticles (AgNP) sensor with magnetic molecularly imprinted polymeric microspheres (Fe3O4@mSiO2@MIPs) as recognition elements. Using Fe3O4 as supporting core, mesoporous SiO2 as intermediate shell, methylacrylic acid as functional monomer, and cartap as template, Fe3O4@mSiO2@MIPs were prepared to selectively and magnetically separate cartap from tea solution before colorimetric determination by AgNP sensors. The core-shell Fe3O4@mSiO2@MIPs were also characterized by FT-IR, TEM, VSM, and experimental adsorption. The Fe3O4@mSiO2@MIPs could be rapidly separated by an external magnet in 10 s with good reusability (maintained 95.2% through 10 cycles). The adsorption process of cartap on Fe3O4@mSiO2@MIPs conformed to Langmuir adsorption isotherm with maximum adsorption capacity at 0.257 mmol/g and short equilibrium time of 30 min at 298 K. The AgNP colorimetric method semi-quantified cartap5 mg/L by naked eye and quantified cartap 0.1-5 mg/L with LOD 0.01 mg/L by UV-vis spectroscopy. The AgNP colorimetric detection after pretreatment with Fe3O4@mSiO2@MIPs could be successfully utilized to recognize and detect cartap residues in tea beverages. © 2018 by the authors.
语种:
英文
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安化黑茶水溶性成分高效液相色谱指纹图谱及定量分析
作者:
王斌;邓慧芸;吴茂;郭亚平;邓斌;...
期刊:
食品科学 ,2017年38(20):125-130 ISSN:1002-6630
通讯作者:
Xie, Lianwu(xiecsu@126.com)
作者机构:
[马强; 谢练武; 邓慧芸; 邓斌; 郭亚平; 王斌; 吴茂] Institute of Applied Chemistry, College of Sciences, Central South University of Forestry and Technology, Changsha, 410004, China;[邓斌] School of Chemical Biology and Environmental Engineering, Xiangnan University, Chenzhou, 423043, China
关键词:
安化黑茶;水溶性成分;指纹图谱;高效液相色谱;化学模式识别
摘要:
目的:运用高效液相色谱(high performance liquid chromatography,HPLC)法研究湖南安化黑茶指纹图谱,并对安化黑茶的主要成分进行定量分析,为湖南安化黑茶的成分分析与鉴别提供理论依据。方法:以22个安化黑茶样品与4种外省黑茶(云南普洱茶、湖北青砖茶、广西六堡茶、四川土司黑茶)为实验材料,采用梯度洗脱(A相为0.17%乙酸溶液,B相为乙腈),柱温30 ℃,检测波长280 nm,流速1.0 mL/min,建立安化黑茶HPLC指纹图谱,并进行了相似度评价与主成分分析,确定共有色谱峰。结果:22个安化黑茶样品具有19个共有色谱峰,这些黑茶样品在共有模式下的相似度为0.783~0.958,而广西六堡茶、四川土司黑茶、湖北青砖茶以及云南普洱茶与安化黑茶相似度很低(<0.3);定量分析表明,安化黑茶中没食子酸、表没食子儿茶素没食子酸酯的含量明显高于4种外省黑茶,而广西六堡茶中的咖啡因和云南普洱茶中的没食子儿茶素含量明显高于安化黑茶;此外,茯砖素A仅在安化黑茶中检出,可作为安化黑茶的标志性成分。结论:根据所构建的安化黑茶HPLC指纹图谱及找到的标志性成分茯砖素A,可用于安化黑茶的鉴定与评价。
语种:
中文
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林业高校化学学科“四层次一体化”研究生创新培养模式
作者:
谢练武;郭亚平;皮少锋;郭鑫;王文磊;...
期刊:
教育教学论坛 ,2017年(41):238-239 ISSN:1674-9324
作者机构:
中南林业科技大学 理学院,长沙,410004;[谢练武; 郭亚平; 黄自知; 王文磊; 郭鑫; 皮少锋] 中南林业科技大学
关键词:
研究生教育;四层次一体化;创新;培养模式
摘要:
为适应创新驱动发展新常态,我院在林业高校化学类研究生课程建设、教学改革理论研究、实验教学内容改革及平台建设、教学团队建设等方面进行系统研究与实践,通过构建新的实践课程体系,进行化学实验课程绿色化改进,逐步形成了林业高校化学学科研究生“四层次一体化”培养新模式。
语种:
中文
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氨基吡啶修饰的高交联树脂合成与吸附性能
作者:
王斌;秦海蛟;皮少锋;谢练武;肖谷清
期刊:
化学研究与应用 ,2016年28(4):525-529 ISSN:1004-1656
作者机构:
中南林业科技大学理学院应用化学研究所, 湖南, 长沙, 410004;湖南城市学院化学与环境工程学院, 湖南, 益阳, 413000;[王斌; 秦海蛟; 皮少锋; 谢练武] 中南林业科技大学理学院应用化学研究所, 湖南, 长沙, 410004;[肖谷清] 湖南城市学院化学与环境工程学院, 湖南, 益阳, 413000
关键词:
氨基吡啶;超高交联树脂;水杨酸;吸附
摘要:
以氯球为原料,二氯乙烷为溶剂,FeCl_3为催化剂,利用Friedel-Crafts反应制备甲苯超高交联树脂,测其氯含量为6.38%。为降低氯含量和提高吸附性能,采用2-氨基吡啶对该高交联树脂进行化学修饰,获得的高交联树脂(记为GQ-08)氯含量下降为1.36%,然后详细研究了GQ-08对水杨酸的吸附性能。实验结果表明, GQ-08在pH 2.75时对水杨酸的吸附容量最大,达到310.7 mg·g~(-1);GQ-08对水杨酸的吸附是放热过程,吸附等温线服从Freundlich方程;当溶液中NaCl含量由0%到2%变化时,GQ-08对水杨酸的吸附量明显减少,说明氯离子与水杨酸存在竞争吸附作用,增加盐度不利于水杨酸吸附。因此,在利用GQ-08树脂进行水杨酸富集分离或处理生产废水回收水杨酸时应优先考虑酸度、盐度等工艺参数。
语种:
中文
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一种氨基吡啶修饰的甲苯超高交联大孔树脂的制备及性能研究
作者:
谢星雨;王斌;秦海蛟;肖谷清;谢练武
期刊:
化学与生物工程 ,2016年33(1):26-29 ISSN:1672-5425
作者机构:
中南林业科技大学理学院应用化学研究所,湖南长沙410004;长沙市第一中学,湖南长沙410005;湖南城市学院化学与环境工程学院,湖南益阳413000;中南林业科技大学理学院应用化学研究所,湖南长沙,410004;湖南城市学院化学与环境工程学院,湖南益阳,413000
关键词:
氨基吡啶;甲苯超高交联大孔树脂;水杨酸;吸附
摘要:
通过傅克烷基化反应,以氯甲基化聚苯乙烯(CMP)与甲苯反应制备氯含量为6.38%的甲苯超高交联大孔树脂GQ-06,然后采用2-氨基吡啶对GQ-06进行化学修饰,制备氯含量为1.36%的甲苯超高交联大孔树脂GQ-08,并比较了CMP、GQ-06与GQ-08对水杨酸吸附性能的差异。结果表明,相较于CMP与GQ-06,GQ-08对水杨酸的吸附大大增强,并在pH=2.75时对水杨酸的吸附量达最大值310.7mg·g(-1),分别是CMP与GQ-06的10.1倍与4.1倍;GQ-08对水杨酸的吸附是放热过程,当溶液中NaCl含量增加时,GQ-08对水杨酸的吸附量明显减少,说明氯离子与水杨酸存在竞争吸附作用。2-氨基吡啶修饰的甲苯超高交联大孔树脂吸附水杨酸存在离子交换吸附和酸碱化学吸附两大吸附机理,吸附容量大,可利用GQ-08树脂处理含水杨酸的生产废水来富集回收水杨酸。
语种:
中文
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