艾蒿柱层析馏分成分分析

将甲苯浸泡获得的艾蒿提取物置于硅土层析柱上,再用乙酸乙酯淋洗获得一个柱层析馏分。用气相色谱对该馏分进行分离,用质谱法和红外光谱法对分离组分进行了结构鉴定。共鉴定出20个纽分,其中倍半萜3个,单萜6个,在这9个萜类组分中,有3个是首次报道。同样,用液相色谱-质谱联用仪(LC—DAD-MSD)对该馏分进行了分析鉴定,结果显示这些组分中可能存在大量的萜类物质。     

离子色谱和热解吸-气相色谱-质谱法测定炸药爆炸产物

用离子色谱和热解吸-气相色谱-质谱法测定炸药的爆炸产物.爆炸产物中的氰化物用0.1 mol·L-1氢氧化钠溶液吸收后,用离子色谱法检测,检出限(3S/N)为0.01 ug·L-1,回收率为92.6%,相关系数为0.999 8,测定结果的相对标准偏差为3.8%.爆炸产物的主成分和微量成分直接进样,用热解吸-气相色谱-质谱联用法分析,检测了联苯、1-甲基-(1H)-吡喏2-乙腈、5-氨基-3,4-二氢-(2H)-吡喏-2-乙腈、硝基苯、苯等有毒产物.     

高效液相色谱-串联质谱法分离鉴定绿原酸及其相关杂质

建立了高效液相色谱-串联质谱法（HPLC-MS/MS)分离和鉴定绿原酸及其相关杂质的方法。采用C18色谱柱(5 μm,4.6 mm×150 mm),乙腈-水（含0.1%甲酸）(体积比为8∶92)为流动相,经HPLC-MS/MS和HPLC-二极管阵列检测器在线检测,对工业绿原酸中的奎尼酸、咖啡酸、绿原酸同分异构体等8个相关杂质的结构进行了鉴定。     

5-甲基吗啡-3-氨基-2-唑烷基酮标准物质的研制

研制了呋喃它酮的代谢产物5-甲基吗啡-3-氨基-2-唑烷基酮(AMOZ)的标准物质.采用红外光谱和液相色谱-质谱法对AMOZ进行了定性鉴定,建立并优化了用于AMOZ主成分定值的高效液相色谱-二极管阵列检测器法(HPLC-DAD)、气相色谱-氢火焰离子化检测器法(GC-FID)和差示扫描量热法(DSC).将卡尔费休法和热...     

顶空固相微萃取-气相色谱-质谱法及模式识别法鉴别群体手部气味

以玻璃珠为采样介质,采用顶空固相微萃取-气相色谱-质谱法分别对不同人体手部气味中主要挥发性成分醇、酚、醛、酮、酸、酯6类物质进行测定。同时采用Kolmorogv-Smirnoff秩检验和Spearman秩相关系数法从定性(共有峰的比率)和定量(共有峰的相对峰面积)的角度,综合地对不同人体气味的色谱图进行统计分析,结果显示,除了酸类和酚类物质不能用作区别不同人体气味的指标性成分外,其他4类物质均可作为鉴别不同人体气味的指标性成分。     

气相色谱-质谱联用结合化学计量学鉴别再生聚苯乙烯发泡餐盒

建立了气相色谱-质谱联用(Gas chromatography-mass spectrometer,GC-MS)结合化学计量学方法鉴别再生餐盒和新餐盒的方法。发泡餐盒试样经二氯甲烷溶解,加入甲醇沉淀大分子聚合物,采用GC-MS进行分析,并结合主成分分析(Principal component analysis,PCA)和正交偏最小二乘判别分析(Orthogonal par-tial least squares discriminantanalysis,OPLS-DA)等多变量统计分析方法筛选出再生餐盒和新餐盒的差异性物质,建立了再生餐盒和新餐盒的鉴别模型。结果表明,再生餐盒和新餐盒中的主要物质包括聚合残余(苯乙烯单体、二聚体和三聚体)、苯衍生物和添加剂等。OPLS-DA和t检验筛选出41种在含量上具有显著性差异的物质,基于差异性物质建立鉴别模型,初步建立了有效的鉴别再生聚苯乙烯发泡餐盒的方法。     

气相色谱质谱法分析土壤中多溴联苯和多溴联苯醚类化合物

建立了气相色谱-质谱法(GC-MS)分析土壤中的18种多溴联苯(PBBs)和多溴联苯醚类(PBDEs)化合物的方法.利用快速溶剂萃取(ASE)技术和凝胶净化系统(GPC)进行土壤样品的前处理,(13)C标记物作为进样内标和替代标,采用电子轰击源气相色谱质谱法(GC-EI/MS )分析-溴至七溴代PBBs和PBDEs,负...     

墨汁粉条的鉴别方法研究

采用气相色谱-质谱(GC-MS)和液相色谱-串联质谱(LC-MS/MS)技术,研究了墨汁粉条(假红薯粉条)及纯正红薯粉条中微量成分的差别。经GC-MS方法检测发现墨汁粉条中含有苯酚、六氢吡咯并[1,2a]吡嗪-1,4-二酮,用LC-MS/MS方法检测发现墨汁粉条中含有人工色素柠檬黄、日落黄和亮蓝,而纯正红薯粉条中不含以上物质。以该5种物质作为特征成分,建立了GC-MS和LC-MS/MS联合鉴别墨汁粉条的新方法。     

超高效液相色谱-质谱联用法与气相色谱-质谱联用法分析水性印油印记的主要成分

应用超高效液相色谱-质谱联用技术(UHPLC-MS)与气相色谱-质谱联用技术(GC-MS),对环保水性印油中的主要成分(主要颜料与挥发性物质)进行了定性分析。通过超声提取与离心对样品进行预处理后,在ZORBAX Eclipse Plus Phenyl-Hexyl (50 mm×4.6 mm, 1.8 μm)液相色谱柱,15 mmol/L乙酸铵水溶液-乙腈为流动相,在UHPLC-MS负离子电喷雾电离条件下以选择离子监测模式定性分析染料及颜料;采用HP-INNOWAX (30 m×0.25 mm, 0.25 μm)气相色谱柱进行GC-MS全扫描,定性分析挥发性物质。研究确认水性印油中的主要颜料成分是酸性红R、水溶曙红Y与颜料红112,主要挥发性物质是甘油、1,2-丙二醇等。本方法快速、准确,可以满足物证鉴定工作中对印记的检测需要,有助于法庭科学中对印油印记的种类区分。     

2,4,6-三氯酚纯品原料纯度定值方法研究

对用于溶液标准物质制备的纯品原料2,4,6-三氯酚纯度定值方法进行了探讨。采用气相色谱质谱法(GC–MS)对主成分和杂质进行定性鉴定。用高效液相色谱法(HPLC–DAD)、气相色谱法(GC–FID)和差示扫描量热法(DSC)3种不同原理的方法对主成分定值。卡尔费休法测量水分,电感耦合等离子体质谱(ICP–MS)测量无机杂质。2,4,6-三氯酚纯度定值结果为99.3%,扩展不确定度为0.6%(k=2)。     

亚铈试纸的设计与制作

以中速定量滤纸作为基纸,依次用作为基纸改性剂的十六烷基三甲基溴化铵(质量分数0.5%)和作为显色剂的二甲酚橙(质量分数0.2%)浸泡、晾干,制成亚铈试纸。 用1.000×10^-5~1.000 mol/L的Ce³⁺标准溶液分别浸泡该试纸,制成11种颜色的标准比色卡。 建立了强酸性Ce⁴⁺/Ce³⁺混合液中Ce³⁺浓度的半定量试纸测定法。 将本法应用于再生电解液和模拟有机合成液中Ce³⁺ 浓度的测定,表明只需用质量分数20%的六次甲基四胺缓冲溶液将试液调整至pH值5.0~6.0,结果准确度良好,共存的Ce⁴⁺、对苯二酚、对羟基苯甲醛、1,10-二羟基蒽醌等组分均不产生干扰。 该试纸具有制作方法简单、廉价易得、检测快速、易操作等优点,可应用于生产流程中Ce³⁺浓度的快速检测。     

A pH optical and fluorescent sensor based on rhodamine modified on activated cellulose paper

A rhodamine‐based colorimetric and fluorescent pH chemosensor ( RhA ) was designed and synthesized via a coupling reaction between rhodamine ethylenediamine and succinic anhydride. RhA showed excellent pH response in aqueous solutions. In addition, common cations (Na⁺, K⁺, Ag⁺, Mg²⁺, Ca²⁺, Pb²⁺, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺, Cd²⁺, Hg²⁺, Al³⁺, Cr³⁺, Fe³⁺, Au³⁺, Pt²⁺, and Ru²⁺) did not interfere with the pH response. As it has the potential to be used as a portable pH sensor, RhA was immobilized on activated cellulose paper using N,N'‐dicyclohexylcarbodiimide (DCC) and N,N'‐dimethylpyridin‐4‐amine (DMAP) as the coupling reagent to obtain a composite pH sensor ( CP‐RhA ). CP‐RhA was characterized by ATR‐FTIR, UV–vis, and fluorescence spectroscopy, and by scanning electron microscopy (SEM). CP‐RhA showed a rapid response in the pH range 1–8 through color and fluorescence changes. DFT calculations showed a blue‐shifted spectrum in the protonated form compared to the neutral form. Moreover, the pH sensor paper could be reused by dipping in NaOH. Thus, our work demonstrates the potential of the rhodamine dye composite for visualizing pH changes in real systems.     

Fast and effective paper based sensor for self-diagnosis of bacterial vaginosis

In this contribution we present a sensitive colorimetric bioactive paper fabricated to determine sialidase-related diseases like bacterial vaginosis (BV) in a one-step and dry format spot assay with fast response and good storage stability. The paper was prepared by three simple steps. The first step involves preparation of poly(ethyleneimine) (PEI) microcapsules, the second step is to incubate positively charged microcapsules in negatively charged 5-bromo-4-chloro-3-indolyl-a-d-N-acetylneuraminic acid (BCIN) solution, a color enhancer nitro blue tetrazolium (NBT), and in the third step, paper was fabricated by incorporating incubated microcapsules into paper pulp. This paper changes color from white to dark purple in the presence of sialidase in as little as 6 min, and color could be enhanced with increased length of reaction time. In this reaction system, BCIN was the substrate for sialidase, NBT was the color enhancer, and PEI microcapsules acted as catalyst. The loading efficiency of BCIN was about 22.2%, and filtered BCIN solution could be reused for the next fabrication.     

Ion Exchange Capacity of Chromatographic Paper

Abstract

The ion exchange capacities of Whatman No. 1 and Whatman CM81 chromatographic papers, with and without pre-washing, were determined chromatographically using lead nitrate and lead chloride. Mean values with standard deviations are reported. Statistical analysis indicates that pre-washing with acetic acid, perchloric acid, and disodium dihydrogen ethylene, diaminetetraacetate affects the capacity by the same amount at the 95% confidence limit.     

利用氧化和希夫碱反应制备具有手性分离功能的滤纸

纸色谱具有微量、快速、高效和灵活程度高等特点。以滤纸为原料用高碘酸钠氧化法合成了二醛基滤纸,通过希夫碱反应接枝手性氨基酸,合成了一种具有手性分离功能的新型纸色谱材料。通过单因素试验和正交试验确定滤纸氧化的最佳合成条件为：高碘酸钠的质量分数为4%, pH值为2,反应温度45℃和反应时间4 h,该条件下氧化滤纸醛基含量为57.93%（物质的量分数）。氧化滤纸与L-谷氨酸通过微波合成得到具有手性分离功能的色谱用纸。利用该种手性滤纸分离外消旋酒石酸,展开剂配方为100 mL 50%正丁醇,50 mL乙酸和0.1000 g溴酚绿。结果显示,L-酒石酸比移值（R_f）为0.52, D-酒石酸R_f为0.40。该方法不需要使用大型设备,适合一般的教学、研究及工业应用。     

石墨烯纸的制备及电容特性

利用未经任何分散处理的氧化石墨溶胶在气-液界面自组装得到氧化石墨纸(ϕ=10 cm), 将氧化石墨纸在不同温度下用水合肼蒸气还原制得石墨烯纸. 采用扫描电子显微镜(SEM)、 X射线衍射(XRD)、 Raman光谱、 X射线光电子能谱(XPS)及氮吸附对还原前后样品的微观结构、 表面特性、 元素组成及比表面积进行了表征, 在此基础上考察了还原处理及还原温度对材料电容特性的影响. 结果表明, 在150 ℃下还原氧化石墨纸得到的石墨烯纸具有较好的电化学电容特性, 其在1000 mA/g恒定充放电电流密度下, 6 mol/L KOH电解质溶液中的质量比电容达到142 F/g, 1000次充放电循环后电容保持率为99.8%.     

A study of cationic glucomannan as a paper strength agent

In this paper, konjac glucomannan was cationized by 3-chloro-2-hydroxypropyl trimethyl ammonium chloride (a kind of cationic reagent) as a paper strength agent. The effects of dosage of cationic reagent, cationization time, cationization temperature and the pH of papermaking on paper properties were analyzed. The results showed that when 1% cationic glucomannan (the cationization temperature was 70°C, dosage of cationic reagent was 20% and cationization time was 5 h) was added, tensile index, burst index and folding endurance of the paper were improved by 11.0%, 13.2%, 72.0%, respectively, compared with the control. The results of SEM analysis, FTIR analysis, and elemental analysis illustrated that the addition of paper strengthening agent make fibers combined more closely, and further lead to the increase of paper strength properties.     

Chromatography Op Primary Aromatic Amines on Cellulose and Carboxymethylcellulose Papers

Abstract

The chromatography of a series of primary aromatic amines is studied on papers composed of pure cellulose and carboxy-methylcellulose with water, acetic acid and an acetate buffer as solvents. Migration data and possible separations are reported, and results are compared with those obtained on carboxymethylcellulose thin layers.     

基于天然聚多糖的环境友好材料（II）-麻纤维和芦苇纤维多元醇的生物降解聚氨酯

以麻纤维和芦苇纤维制备的植物多元醇为原料,合成具有良好性能的生物降解 性硬质聚氨酯泡沫体,其密度40 kg/m~3左右,压缩强度150 kPa,弹性模量4 MPa 。而且多元醇中植物原料含量越大,其性能越好,这使植物原料的充分利用和材料 生产成本的降低成为可能。土壤掩埋实验表明,泡沫体有很好的土壤微生物降解性 。     

反相纸层析与液液萃取

本文探讨了反相纸层析与液液萃取的关系,首先对Cerrai,E.提出的萃取色层两种滞留机制的理论,即离子交换与分配机制,提出不同的看法。认为q=1的现象是As变化的结果而与机制无关。本文认为当固定相为液体或溶液时,反相纸层析与液液萃取一样属于分配机制。这样反相纸层析对萃取工作可以提供有益的信息,它的R_f图谱可以作为一种简便地、快速地筛选萃取剂的工具。此外选择适当的条件,它还可以用来研究萃取机理。