满山白化学成分的研究

满山白系杜鹃花科植物毛果杜鹃(Rhododendron seniavinii Maxim.).福建省建阳地区用其根和叶治疗慢性气管炎千余例,对止咳、祛痰均有较好的疗效.有关满山白化学成分的研究国内外尚未见报道,为进一步阐明其有效成分,进行了化学成分的研究.     

青海杜鹃挥发油化学成分的研究

应用含硝酸银的氧化铝柱层析等方法,从青海杜鹃(Rhododendron Tsinghaiense Ching.)挥发油中有效地分得21个化合物,并经紫外光谱、红外光谱、核磁共振谱、质谱、气相层析和化学方法等测得其中17个化合物分别为1～17.药理筛选结果表明,其中δ-杜松烯、γ-杜松烯、异愈创木醇和α-杜松醇具有祛痰作用;愈创木醇和异愈创木醇具有镇咳作用.     

杜鹃素Ⅱ的二维NMR谱研究

在我们开展对国产杜鹃花科植物所含二萜类活性物质的研究中,从羊踯躅(Rhododen-dron Molle G.Don)的花中分得一种成份,经波谱等手段测定,证实为已知的杜鹃素Ⅱ(Rhoaojaponin Ⅱ)。据报道,此类成份在临床上具有速降血压和抗心动过速的功效。为了对此类物质进行药物构效关系及结构改造研     

香格里拉产小叶杜鹃花挥发性成分的GC-MS分析

研讨香格里拉县小叶杜鹃花的挥发油化学成分,为进一步合理开发利用其药用资源提供试验依据。利用水蒸汽同时蒸馏萃取法(SDE)提取小叶杜鹃花的挥发性化学成分,通过气相色谱-质谱联用技术(GC-MS)对各个色谱峰定性,并采用色谱峰面积归一法获得各个化合物的相对含量。从小叶杜鹃花挥发油中共分离鉴定了73个色谱峰,占挥发油总量的85.53%。小叶杜鹃花挥发油主要成分有α-蒎烯(14.00%)、正二十三烷(9.51%)、7-甲氧基-2,2-二甲基-3-色烯(6.26%)、正二十烷(6.11%)、苯乙醇(5.10%)、1-Heneicosyl formate(4.60%)等。     

大孔树脂-高速逆流色谱法分离纯化地黄中毛蕊花糖苷（英文）

该文建立了大孔树脂-高速逆流色谱分离中药材地黄中有效成分毛蕊花糖苷的方法。考察了4种大孔树脂对地黄粗提物中毛蕊花糖苷的静态吸附与解吸情况,其中D101大孔树脂对目标成分的吸附率与解吸率最理想,实验结果表明体积分数为10%的乙醇洗脱得到的毛蕊花糖苷含量最高,目标成分含量从4.9%提高到32.6%。最后,部分纯化的样品(165 mg)采用高速逆流色谱进一步纯化,两相溶剂系统由乙酸乙酯-正丁醇-水(1∶4∶5,v/v/v)组成,分离得到45 mg纯度为96%的毛蕊花糖苷。     

大孔树脂-高速逆流色谱法分离纯化地黄中毛蕊花糖苷

该文建立了大孔树脂-高速逆流色谱分离中药材地黄中有效成分毛蕊花糖苷的方法。考察了4种大孔树脂对地黄粗提物中毛蕊花糖苷的静态吸附与解吸情况,其中D101大孔树脂对目标成分的吸附率与解吸率最理想,实验结果表明体积分数为10%的乙醇洗脱得到的毛蕊花糖苷含量最高,目标成分含量从4.9%提高到32.6%。最后,部分纯化的样品（165 mg）采用高速逆流色谱进一步纯化,两相溶剂系统由乙酸乙酯-正丁醇-水（1：4：5,v/v/v）组成,分离得到45 mg纯度为96%的毛蕊花糖苷。     

高效液相色谱法快速测定满山红中槲皮素和杜鹃素的研究

研究了用固相萃取预分离,高效液相色谱法测定满山红中槲皮素和杜鹃素。槲皮素和杜鹃素用90%甲醇加热回流提取,提取液用Waters Sep-Pak-C18固相萃取小柱预分离,然后用ZORBAX Stable Bound(50×4.6 mm i.d.,1.8μm)色谱柱,以0.2%的磷酸和甲醇(52∶48,V/V)为流动相,槲皮素和杜鹃素在1.0 min内可达到基线分离;用紫外二极管矩阵检测器检测。方法的加入标准回收率为98%~102%,相对标准偏差为1.6%~1.8%。本法可用于满山红样品中的槲皮素和杜鹃素的测定,结果满意。     

基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测

建立了利用超高效合相色谱法(Ultra performance convergence chromatography,UPC2)快速分离和测定黄芪中5种主要黄酮类化合物(毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷、芒柄花素)的方法.黄芪样品采用80％乙醇提取后,以超临界CO2-0.2％ H3PO4-甲醇溶液为流动相,梯度洗脱,色谱柱为Waters ACQUITY UPC2 CSH柱(100 mm×3.0 mm,1.8 μm),柱温为40℃,流速为0.4 mL/min,进样量为1μL,检测波长为280 nm.整个分析过程仅需15 min,分析速度是传统液相色谱的3倍以上.结果表明:毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷与芒柄花素的检出限及定量限范围分别在0.3 ～0.5 mg/kg和1.0～2.0 mg/kg之间,5种黄酮类成分的加标平均回收率均高于99.7％,相对标准偏差(RSD)小于2.2％(n=6);在最优条件下,对13批不同产地的黄芪进行检测,毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷与芒柄花素的含量范围分别在4.8 ～ 102 mg/kg、14 ～ 277 mg/kg、0 ～ 135 mg/kg、5.3 ～ 119 mg/kg及2.8 ～ 41 mg/kg之间;本方法简便快速,重复性良好,结果准确可靠,可用于黄芪药材中5种主要黄酮类成分的含量测定.     

中药材黄芪与红芪的色谱鉴别法

目的：鉴别中药材黄芪和红芪．方法：高效液相色谱法,数据分析用waters公司．Patten Mattch软件．结果：黄芪和红芪药材的区别是在高效液相色谱指纹图谱中黄芪药材有26个特征峰,红芪药材有23个特征峰;红芪中毛蕊异黄酮的含量低于芒炳花素,黄芪中毛蕊异黄酮的含量高于芒炳花素;红芪中不含黄芪甲苷,黄芪中含有黄芪甲苷．结论：可以用色谱法准确、可靠地鉴别黄芪和红芪药材．     

高效液相色谱法研究红芪指纹图谱

研究了10个红芪样品的指纹图谱,采用高效液相色谱法,乙腈-水梯度洗脱,流速1．0mL／min,柱温25℃,色谱图光谱采集范围：190～400nm,以武都米仓山红芪药材作为对照品,用指标成分毛蕊异黄酮和芒柄花素进行了定位,并测定了它们的含量,找出了23个共有峰,其中10号峰和14号峰分别为毛蕊异黄酮和芒柄花素。10个样品平均相似度为97．3％以上,结果表明：红芪样品指纹图谱及指标成分含量测定可用于全面控制红芪药材的质量。     

Fluorimetric and mass spectrometric study of the interaction of beta-cyclodextrin and osthole

The inclusion complex of beta-cyclodextrin (beta-CD) and osthole was studied by the electrospray ionization mass spectrometry (ESI-MS) and fluorescence spectrometry. From the mass spectrum, the 1:1 stoichiometric inclusion complex of beta-CD and osthole was observed. The tandem mass spectrum was performed. The fluorescence intensity of osthole increased in the present of beta-CD. According to the 1:1 beta-CD-osthole mode, the dissociation constant (KD) was obtained by ESI-MS and fluorescence spectrometry. The KD of beta-CD-osthole inclusion complex is 6.96 x 10(-3) mol L(-1) obtained by mass spectrometry and that is 8.14 x10 (-3) mol L(-1) obtained by fluorescence spectrometry, which is consistent with each other.     

Characterization of the mycotoxin fumonisin B1: comparison of thermospray, fast-atom bombardment and electrospray mass spectrometry.

The utility of thermospray mass spectrometry (TSMS), fast-atom bombardment mass spectrometry (FABMS), and electrospray mass spectrometry (ESMS) for the analysis of Fumonisin B1 is investigated. In addition, the analysis of two different standards of Fumonisin B1 as well as an inoculated corn culture extract that contained Fumonisin B1 is reported. The results of these efforts show that ESMS, as well as FABMS and a combination of FAB and tandem mass spectrometry (FABMS/MS), provide useful data for the characterization of Fumonisin B1. The detection limit was 50 pg for Fumonisin B1 when analyzed by full scan FABMS, and 5 pg when analyzed by single-reaction monitoring FABMS/MS.     

Synthesis of chromophoric crown-containing styryl derivative of terthiophene and its complexation with octane-1,8-diaminium diperchlorate

2,2′: 5′,2″-Terthiophene derivative containing benzo-18-crown-6 fragments linked through ethene spacers was synthesized, and its complexation with octane-1,8-diaminium diperchlorate in acetonitrile was studied by spectrophotometric titration, ¹H NMR, and mass spectrometry. The 1: 1 stoichiometry of the complex was confirmed by mass spectrometry, and its structure was proposed on the basis of the ¹H NMR data.     

原子荧光法检验环境空气中汞的含量

目的采用原子荧光法检验环境空气中汞的含量。方法建立微波消解-原子荧光法,研究微波消解前处理效果,并进行精密度、准确度以及样品实验。结果样品空气中汞的含量为1.44、1.09、1.82 ng/m~3。结论原子荧光法检验环境空气中汞的含量前处理简单,样品消解完全,回收率高。     

Trace characterization of high-purity molybdenum and tungsten by electrothermal atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry and total reflection X-ray fluorescence spectrometry involving analyte—matrix separation

A technique for the separation of 42 trace elements from up to 5 g of molybdenum and tungsten matrices was developed by means of the radiotracer technique. It is based on adsorption of the analyses on the cation exchanger Dowex 50 W x 9 from a 4% H₂O₂/0.01 mol 1⁻¹ HNO₃ solution followed by their elution with 15 ml of 4 mol I⁻¹ HNO₃ in the opposite flow direction. Both matrices were removed with a separation factor > 10⁴. The separation technique was applied to the analysis of these materials by electrothermal atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry and total reflection X-ray fluorescence spetrometry. For all the determination methods used, the limits of detection are given and compared with those of other methods. With inductively coupled plasma mass spectrometry, for 22 of the 30 assayed elements, limits of detection at the sub-ng g⁻¹ level were achieved. The results are compared with those obtained by radiochemical neutron activation analysis in this work and by glow discharge mass spectrometry, secondary ion mass spectrometry, isotope dilution mass spectrometry and by solution spectrometric methods in other laboratories.     

Determination of arsenic in gold by flow injection inductively coupled plasma mass spectrometry with matrix removal by reductive precipitation

Arsenic was determined in gold by flow injection hydride generation inductively coupled plasma-mass spectrometry following a batch mode reductive precipitation removal of the interfering gold matrix. A solution of potassium iodide, L-ascorbic acid, and hydrochloric acid was used as the reluctant. The recovery of gold by precipitation and filtration was 99 ± 3%. The detection limit for arsenic in gold was 55 ng g⁻¹ in the solid. The concentration of arsenic that was determined in the Royal Canadian Mint gold sample FAU-10 was 29.7 μg g⁻¹ in the solid; this value was indistinguishable, with 95% confidence, from values determined at the Royal Canadian Mint by graphite furnace atomic absorption spectrometry and by inductively coupled plasma-mass spectrometry. The standard deviation for four replicate determinations of the arsenic in FAU-10 was 0.972 μg g⁻¹ in the solid.     

三尖杉酯碱侧链酸的不对称合成及结构表征

以N-Boc苏氨醛为起始原料,经Wittig、Meisenheimer重排和催化氢化系列反应,不对称合成了天然产物三尖杉酯碱的侧链酸,中间体及目标产物结构经核磁共振(1 H NMR、13 C NMR)、红外光谱和质谱表征.结果表明,所用合成方法具有产率高、反应条件温和、操作简单等优点;目标化合物的总收率达30%.     

手性联萘酚的多胺缀合物的合成与表征

以N1-氨基丁基-N1,N4-二叔丁氧羰基-1,4-丁二胺和手性甲酰基联萘酚为原料,经缩合后用NaBH4还原,产物提纯后脱保护,得到目标产物S-6和R-6,所得化合物的结构均经IR、1H NMR、13C NMR和MS测试确认.     

Performance of alpha spectrometry in the analysis of uranium isotopes in environmental and nuclear materials

The accuracy of alpha spectrometry in the determination of uranium isotopes at various concentrations levels and with various isotope ratios was tested in a round robin international intercomparison exercise. Results of isotope activity/mass and isotope mass ratios obtained by alpha spectrometry were accurate in a wide range of uranium masses and in isotopic ratios typical of depleted, natural, and low enriched uranium samples. Determinations by alpha spectrometry compared very satisfactorily in accuracy with those by mass spectrometry. For example, determination of U isotopes in natural uranium by alpha spectrometry agreed with mass spectrometry determinations at within ±1%. However, the ²³⁶U isotope, particularly if present in activities much lower than ²³⁵U, might not be determined accurately due to overlap in the alpha particle energies of these two uranium isotopes.     

手性化合物的质谱分析研究

运用不含手性碳的非对称化合物Ｓ－ＢＮＰ酸（Ｓ－ｐｈｏｓｐｈｏｒｓａｅｕｒｅ－（１，１＇－ｂｉｎａｐｈｔｈｙｌ－２，２＇－ｄｉｙｌｅｓｔｅｒ））作反应试剂用快原子轰击反应质谱法（ＦＡＢ－ＲＭＳ）测定手性化合物的绝对构型．发现非对称手性化合物可与不对称手性化合物在质谱中发生立体选择性反应，Ｓ－ＢＮＰ酸可作为一种新的反应试剂来测定手性化合物的绝对构型．