HPLC指纹图谱应用于炙甘草的炮制研究

目的:应用HPLC指纹图谱规范炙甘草的炮制。方法:采用反相高效液相色谱法,DENALI C18色谱柱(VYDAC238DE5415,120A,5μm,4.6mm×150mm),以3%(v/v)HAc溶液和甲醇为流动相,梯度洗脱,柱温40℃,检测波长252nm。结果:炙甘草的HPLC指纹图谱有20个共有峰。传统炒制法炮制的炙甘草样品有一部分峰的重现性RSD值>3%;烘制法炮制的样品重现性有2个共有峰相对峰面积比的RSD>3%;微波法炮制的样品重现性符合指纹图谱的要求,20个共有峰相对峰面积比的RSD值均小于3%。结论:烘制和微波加热的炮制方法,可控性强,样品的指纹图谱重现性高,可以作为替代传统炒制工艺的新工艺。国家自然科学基金2003重点项目(20235020

Determination of Glycyrrhizin and Liquiritin in Licorice(Glycyrrhiza) by HPLC Method

目的测定甘草中甘草酸和甘草苷的含量。方法采用反相高效液相色谱法,DENALIC18色谱柱(VYDAC238DE5415,120A,5μm,4.6 mm×150 mm),梯度洗脱,流动相A∶H2O,流动相B∶1.5%HAc-M eOH,流速1.0 m.lm in-1,检测波长在32.2 m in从330 nm换为252 nm,从35 m in换为330 nm,柱温40℃。结果甘草苷的浓度在10~50μg.m l-1之间与峰面积线性关系良好,平均回收率为99.97%,方法精密度RSD=0.12%(n=5),甘草酸的浓度在50~90μg.m-l1之间与峰面积线性关系良好,平均回收率为100.25%,方法精密度RSD=0.13%(n=5)。结论该方法可用于甘草中甘草酸和甘草苷的同时含量测定。ObjectiveTo determine the content of glycyrrhizin and liquiritin in licorice(Glycyrrhiza).MethodsRP-HPLC method was estabilished.The analytical column was DENALI C18(VYDAC 238DE5415,120A,5μm,4.6 mm×150 mm),and gradient elution with A:H_2O,B:1.5% HAc-MeOH as mobile phase.The flow-rate was 1.0 ml·min~(-1).The detection wavelength was from 330nm to 252 nm at the 32.2 min,and then returned to 252 nm at the 35 min.The column temperature was 40℃.ResultsThe content of liquiritin was good linear related to its peak area in range of 10～50 μg·ml~(-1),and the average recovery of the method was 99.97%,the RSD of precision test was 0.12%(n=5).The content of glycyrrhizin was good linear related to its peak area in range of 50～90 μg·ml~(-1),and the average recovery of the method was 100.25%,the RSD of precision test was(0.13)%(n=5).ConclusionThe method can be used for determing the content of glycyrrhizin and liquiritin in licorice at the same time.国家自然科学基金2003重点项目(No.20235020

Discussion on the Feasibility Applied Fingerprint Chart in Quality Control of Chinese Herbs Pieces

　为促进中药饮片质量的研究,通过对文献资料的归纳、分析,对应用各种方法建立中药标准炮制品的指纹图谱库,并以指纹图谱相似度来评价中药饮片质量的可行性进行综合评述。中药指纹图谱在实现对中药饮片进行科学、客观、公正、有效的质量控制方面将起到重要的作用。In order to promoting the quality research of Chinese herbs pieces, the authors summed up and analyzed many literature information, and synthetically commented the feasibility applied the similarity of fingerprint chart in quality control of Chinese herbs pieces. It would show a important effect in impersonally and effectively controlling the quality of Chinese herbs pieces

Effect of Substituents of Amines on Electrochemiluminescence of Tri(2,2′-bipyridine)ruthenium with Some Amines

研究了苦豆子中主要生物碱槐定碱、苦参碱 ,以及神经兴奋药物甲基安非他命、安非他命等化合物 ,在碱性联吡啶钌 [Ru(bpy) 3 2 + ]水溶液 (pH 9 0 )中的电致化学发光 (ECL)行为 .在玻碳电极上 ,生物碱中的氨基氮于 +1 30V(vs .Ag/AgCl)左右被氧化为氮正自由基离子 ,该自由基离子与Ru(bpy) 3 2 + 反应生成激发态的Ru(bpy) 3 2 + 而发光 .研究比较了取代基性质、氨基氮周围的三维空间结构对各生物碱ECL的影响 ,并结合生物碱氨基氮的电离势和键角的计算 ,对这些影响进行了解释 .Electrochemiluminescences (ECLs) based on tris(2,2′-bipyridine)ruthenium (Ⅱ) [Ru(bpy) 3 2+] and some alkaloids or amines such as sophoridine, matrine, methamphetamine and amphatamine in phosphate buffer solution (pH 9.0) are studied. The light emission is mainly caused by the electro-oxidation reaction between amino group on the alkaloid compounds and Ru(bpy) 3 2+ in a thin layer flow cell equipped with a glassy carbon disc electrode (22.1 mm 2) at about the potential of +1.30 V (vs. Ag/AgCl). The luminescence wavelength of 610 nm confirms that ECL is caused by Ru(bpy) 3 2+* back to its ground state. The effects of the nature and three-dimensional conformation of the substituents of these alkaloids on the ECL intensities are discussed. Ionization potentials and angle of C-N-C bond taken from calculation data further confirm the experimental results.国家自然科学基金 (No .2 98770 2 2 )资助项

Effect of substituents of amines on electrochemiluminescence of tri(2,2 '-bipyridine) ruthenium with some amines

Electrochemiluminescences (ECLs) based on tris(2,2'-bipyridine) ruthenium (II) [Ru(bpy)(3)(2+)] and some alkaloids or amines such as sophoridine, matrine, methamphetamine and amphatamine in phosphate buffer solution (pH 9.0) are studied. The light emission is mainly caused by the electro-oxidation reaction between amino group on the alkaloid compounds and Ru(bpy)(3)(2+) in a thin layer flow cell equipped with a glassy carbon disc electrode (22.1 mm(2)) at about the potential of + 1.30 V ( vs. Ag/AgCl). The luminescence wavelength of 610 nm confirms that ECL is caused by Ru(bpy)(3)(2+*) back to its ground state. The effects of the nature and three-dimensional conformation of the substituents of these alkaloids on the ECL intensities are discussed. Ionization potentials and angle of C-N-C bond taken from calculation data further confirm the experimental results

Synthesis of magnetic, fluorescent and mesoporous core-shell-structured nanoparticles for imaging, targeting and photodynamic therapy

通讯作者地址: Chen, XL (通讯作者),Xiamen Univ, Coll Chem & Chem Engn, State Key Lab Phys Chem Solid Surfaces, Xiamen 361005, Peoples R ChinaA synthetic method to prepare novel multifunctional core-shell-structured mesoporous silica nanoparticles for simultaneous magnetic resonance (MR) and fluorescence imaging, cell targeting and photosensitization treatment has been developed. Superparamagnetic magnetite nanoparticles and fluorescent dyes are co-encapsulated inside nonporous silica nanoparticles as the core to provide dual-imaging capabilities (MR and optical). The photosensitizer molecules, tetra-substituted carboxyl aluminum phthalocyanine (AlC(4)Pc), are covalently linked to the mesoporous silica shell and exhibit excellent photo-oxidation efficiency. The surface modification of the core-shell silica nanoparticles with folic acid enhances the delivery of photosensitizers to the targeting cancer cells that overexpress the folate receptor, and thereby decreases their toxicity to the surrounding normal tissues. These unique advantages make the prepared multifunctional core-shell silica nanoparticles promising for cancer diagnosis and therapy.NSFC21021061,20925103,20871100,Fok Ying Tung Education Foundation 121011 NSF of Fujian Province 2009J06005 Fundamental Research Funds for the Central Universities 2010121015 Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministr

CCCCC pentadentate chelates with planar Möbius aromaticity and unique properties

本课题充分发挥了厦门大学多学科协同研究优势，通讯作者为夏海平教授（合成、表征）、刘刚教授（生物医学应用）和吕鑫教授（理论计算）。合成实验和结构表征由朱从青（第一作者，目前在麻省理工学院、2005年诺贝尔化学奖得主Richard Schrock教授课题组从事博士后研究）完成；生物医学应用由杨彩霞（共同第一作者）、林凎、杨宇惠、王晓勇合作完成；理论计算由朱军、王永恒、朱从青完成。美国NIH的陈小元教授参与了生物医学应用的讨论。该研究工作得到国家自然科学基金委、科技部项目的支持。The coordinating atoms in polydentate chelates are primarily heteroatoms. We present the first examples of pentadentate chelates with all binding atoms of the chelating agent being carbon atoms, denoted as CCCCC chelates. Having up to five metal-carbon bonds in the equatorial plane has not been previously observed in transition metal chemistry. Density functional theory calculations showed that the planar metallacycle has extended Craig-Möbius aromaticity arising from 12-center–12-electron dπ-pπ π-conjugation. These planar chelates have broad absorption in the ultraviolet-visible–near-infrared region and, thus, notable photothermal performance upon irradiation by an 808-nm laser, indicating that these chelates have potential applications in photothermal therapy. The combination of facile synthesis, high stability, and broad absorption of these complexes could make the polydentate carbon chain a novel building block in coordination chemistry.the National Basic Research Program of China (nos. 2012CB821600 and 2014CB744503) , the National Science Foundation of China (nos. 21332002, 81422023, 51273165, 21490573, and 21573179)

Electrochemical Gating Single-Molecule Circuits with Parallel Paths

# These authors contributed equally to this work.电化学门控已成为一种可行且高效调节单分子电导的方法。在本研究中,我们证实了具有两个平行苯环的单分子电路中电子传输可以通过电化学门控控制。首先,我们利用STM-BJ技术以金为电极构筑了具有两条平行路径的单分子结。与单条路径的单分子结相比,两条路径的分子结由于具有增强性量子干涉效应,具有2.82倍的电导值。进一步地,我们利用电化学门控对具有两个平行苯环的单分结的电导进行调控,获得了333%·V-1调节比。结合DFT计算,发现在E=EF附近的V形透射系数谱图导致了实验观测的电导门控行为。本研究揭示了具有平行路径的单分子电路的电化学门控行为,并为设计高性能分子器件的分子材料提供了新的途径。通讯作者:周小顺E-mail:[email protected]:Xiao-ShunZhouE-mail:[email protected].浙江师范大学物理化学研究所,先进催化材料教育部重点实验室,浙江 金华 3210042.上海大学物理系,上海 2004441. Key Laboratory of the Ministry of Education for Advanced Catalysis Materials, Institute of Physical Chemistry, Zhejiang Normal University, Jinhua 321004, Zhejiang, China2. Department of Physics, Shanghai University, Shanghai 200444, Chin

改良分子信标-双重实时荧光PCR快速检测SARS病毒

目的建立改良分子信标-双重实时荧光PCR检测SARS病毒的方法,用于SARS的早期诊断和动物溯源。方法利用改良分子信标技术、装甲RNA和双片段双色荧光技术,根据GenBank公布的SARS病毒聚合酶基因1b的阅读开放框架结构的保守序列,自行设计一对引物和探针,以部分临床标本的酶联吸附实验结果和传统细胞培养方法作为对照,建立分子信标检测SARS病毒的方法。对368份临床标本(咽漱液、血液、粪便、尿液)、52份细胞培养液和50份动物标本进行荧光PCR扩增。结果分子信标检测SARS病毒的方法灵敏度为10～100个拷贝ml,与流感病毒等呼吸道病毒无交叉反应。分子信标检测368份临床标本,20份阳性。其中确诊病例阳性率为21.27%(1047),确诊病例的咽漱液阳性率为43.48%,还分别从粪便和血清中检测到SARS病毒。52份细胞培养液,29份阳性,阳性率为55.77%。50份动物标本,23份阳性,阳性率为46%。结论改良分子信标-双重实时荧光PCR检测SARS病毒方法灵敏度高、特异性强,可用于SARS的临床早期诊断和动物溯源

良渚遺跡群の研究

良渚囲壁は東西南北の4面にそれぞれ2門が開く構造であることが判明した。内外両側に環濠を配しており、いわゆる水城の様相を呈している。囲壁内部のほぼ中央に位置する莫角山土台の基底部に積まれた「土嚢」の年代測定から、莫角山の建造が紀元前2900年前後にまでさかのぼることが確認された。遺跡群西方では崗公嶺地点を初め何か所かでダム状遺構が検出されており、これまた紀元前3000年頃に位置づけられる。塘山土塁とともに複雑な水利施設群を構成していたことが明らかとなった。Liangzhu enclosure is rectangular in shape and each side has two gates. The wall is accompanied by inner and outer moats, so it may have seemed like a ‘floating city’. Mojiaoshan platform, which is located at the center of the enclosure, is dated back to around 2900BC from the carbon-14 dating of the sandbags of vegetable matter piled near the bottom of the platform. To the west of Liangzhu site groups, some dam-like earthen structures have been found such as Ganggongling site and they are also dated back to 3000BC. It is clear they consisted complicated hydraulic facilities together with Tnagshan rampart.出典：研究課題「中国における都市の生成: 良渚遺跡群の学際的総合研究 / Urban Genesis in China: Multidisciplinary Study of Liangzhu Site Groups」課題番号22251010（KAKEN：科学研究費助成事業データベース（国立情報学研究所））（https://kaken.nii.ac.jp/report/KAKENHI-PROJECT-22251010/22251010seika/）著者版報告書の全文を掲載、報告書目次を再掲