反相高效液相色谱法测定辣椒果实中辣椒素含量

１引言辣椒是我国广泛栽培的蔬菜作物，品种多，资源丰富，为了对大批辣椒品种资源进行辣味品质鉴定，需建立快速测定辣椒果实中辣椒素（ｃａｐｓａｉｃｉｎ）含量的方法。在国内，辣椒素的测定一般采用分光光度法，但该方法的样品前处理繁琐，且灵敏度较低。应用反相高效液相色谱法进行辣椒素的定量分析在国内尚未见报道，本文对辣椒果实中辣椒素的卒取及色谱分离条件进行了探讨，得到了满意的分离效果。２实验部分２．１仪器与试剂Ｖａｌｌａｎ５０００型高效液相色谱仪，ＵＶ－１００可变波长紫外检测器，ＣＤＳ４０１数据处理系统。辣椒…     

大孔吸附树脂对辣椒素类物质的富集

辣椒;辣椒素;辣椒素类物质;吸附树脂;分离     

简便连续加压柱层析

简便连续加压柱层析蒲含林，汪波，朱可佳，郑其煌（中山大学化学系，广州５１０２７５）柱层析是有机合成，天然产物（化学等研究）中经常使用的一种分离提纯手段。实验室中，经常用的柱层析分离方法有３种：一是常压柱层析，洗脱剂依靠重力将混合物中各组分依次洗脱下来...     

辣椒素酯类物质的酶促合成

天然辣椒素酯类物质(Capsinoids)是从日本的一种甜椒中分离得到的结构类似辣椒的酯类物质[1,2],包括辣椒素酯(Capsiate)、二氢辣椒素酯(Dihydrocapsiate)及降二氢辣椒素酯(Nordihydro-capsiate),为相对应的辣椒素的脂肪酰基与香草醇形成的酯类化合物(结构如图1)。无辣味,生物活     

离子交换树脂CM—FF在神经生长因子分离,纯化中的应用

本文采用国产阳离子交换树脂CM－FF，两步柱层析从小鼠颌下腺中分离、纯化神经生长因子（β-NGF），并与Whatman公司的CM-C（CM32）离子交换树脂进行了比较。结果表明：CM－FF吸附β－NGF的最适pH分别为6．8和40，最佳流速：柱Ⅰ0．5ml／min，柱Ⅱ0．3ml／min，最佳解析剂为含0．4mol／LNaCl的pH9．0的Tris-HCl缓冲液。CM-FF每克可吸附小鼠颌下腺粗蛋白3-4g，最终纯化得β-NGF2－3mg。CM－FF在分离、纯化β－NGF的应用效果与CM－32是基本相同的，可以替代或至少部分替代CM-32，用于β-NGF的分离、纯化。     

一种新型含磷极压剂的组成与结构研究

采用溶剂萃取和柱层析的分离方法，使用红外光谱、核磁共振、质谱（包括ＥＩ－ＭＳ、ＦＤ－ＭＳ、ＦＡＢ－ＭＳ）等现代 仪器分析技术，对高档齿轮油复合添加剂的主剂——含磷极压剂的组成和结构进行了较为详尽的分析和研究，其 化学结构为硫代磷酸二己脂十二胺盐。     

超高效液相色谱法快速测定辣椒素类物质

建立了超高效液相色谱法快速测定辣椒制品中辣椒素、二氢辣椒素、降二氢辣椒素的方法.样品以四氢呋喃-甲醇(体积比1:1)提取,采用反相高效液相色谱分离.色谱柱为BEH C18,流动相乙腈-水进行梯度洗脱;二极管阵列检测器(DAD),检测波长为280 nm.各成分在1.0 -100.0 mL/L范围内线性良好.辣椒素、二氢辣...     

液-液萃取-液相色谱-串联质谱法测定“地沟油”中辣椒碱类化合物及丁香酚

建立了“地沟油”中辣椒碱类化合物(包括辣椒素、二氢辣椒素、合成辣椒素)及丁香酚的液-液萃取及液相色谱-串联质谱(LC-MS/MS)检测方法。“地沟油”中辣椒碱类化合物及丁香酚用甲醇萃取,采用SUPEL COSIL ABZ+Plus dC18色谱柱(150 mm×4.6 mm, 5 μm)分离,电喷雾离子源在正、负离子模式下电离,多反应监测(MRM)模式扫描。对辣椒素、二氢辣椒素、合成辣椒素及丁香酚的检出限分别为0.02、0.03、0.03和0.6 μg/L,且在一定的质量浓度范围内线性良好。同一操作人员与不同操作人员间测定的精密度低于5%。该方法专属性强、灵敏、准确,可以作为“地沟油”的判定标准之一。     

对辣椒色素某些性能的测试

对辣椒色素某些性能的测试陈连文（河北经贸大学轻工系石家庄０５００６１）刘敬兰（河北师范大学实验中心石家庄０５００１６）关键词分离辣椒色素测定红辣椒属茄科，辣椒属（ＣａｐｓｉｃｕｍｆｒｕｔｅｓｃｅｎｓＬ．），我国各地均有栽培，品种多，资源丰富。内服有开...     

[Co(N-(2-Aminoethyl)-1,3-propanediamine)(1,2-diamino-2-methylpropane)Cl][ZnCl4]配合物部分异构体的结构解析

利用过氧化物合成－分解法制备得到一新的「Ｃｏ（Ｎ－（２－Ａｍｉｎｏｅｈｙｌ）－１,３－ｐｒｏｐａｎｅｄｉａｍｉｎｅ）（１,２－ｄｉａｍｉｎｏ－２－ｍｅｔｈｙｌｐｒｏｐａｎｅ）Ｃｌ」＾２＋体系配合物,并用柱层析分离得到部分几何异体,用单晶Ｘ－射线衍射分析方法解析了其中一反式（三元胺仲氮上的氢相对于Ｃｌ）经式异构体的晶体结构,用二维核磁共振技术的同核质子相关ｇＣＯＳＹ及ＮＯＥＳＹ谱解析了其中一顺式（三元胺仲氮上的树相对于Ｃｌ）经式异构体在溶液中的结构。     

环丁砜与某些碳八芳烃分子络合作用的研究

本文用气液色谱法及混合过程体积的变化研究C₈芳烃与环丁砜的分子络合作用,用参考柱法和混合柱法测定了五种C₈芳烃与环丁砜的络合常数,研究了C₈芳烃与环丁砜和丙二醇-1,2-碳酸酯的二元系超额体积,环丁砜与五种C₈芳烃构成的体系均有强烈的体积收缩效应,苯乙烯与环丁砜体系尤其明显,芳烃与丙二醇-1,2-碳酸酯构成的体系收缩程度远远低于前者。     

腈菌唑分子印迹聚合物的制备及识别性能研究

以腈菌唑为模板分子，采用原位分子印迹技术，制备具有特定识别性能的连续棒状分子印迹聚合物。考察了流动相中酸量对分离的影响，研究了几种结构类似物在所得分子印迹柱上的保留特性。结果表明，这种棒状分子印迹聚合物比相应的空白聚合物有高的识别性能和选择性。     

离子色谱固定相最新进展

介绍离子色谱固定相的最新研究进展。离子色谱固定相在多种类型、含多种功能基和高交换容量固定相,羟基选择性固定相,高效的涂覆型固定相,可变交换容量的固定相,静电离子和仿生离子固定相,整体式固定相。以及芯片式固定相等方面均有所发展。     

高分子色谱固定相GDX203的改性及其在色谱分离中的应用

通过对高分子色谱固定相GDX 2 0 3的硝化改性处理 ,得到新型色谱固定相改性GDX 2 0 3.该固定相用于甲醇羰基合成醋酸的反应产物分析 ,可在恒温条件下快速分离反应介质中的全部组分 ,尤其是乙酸甲酯和碘甲烷可得到完全分离     

L-脯氨酸衍生物为手性侧链的新型C_2对称型手性固定相

绕轴旋转180°能与自身重合的C_2对称型手性化合物在手性催化和手性分离领域有重要应用。以L-脯氨酸苯基酰胺衍生物为手性源,合成了一类新型的C_2对称型手性固定相,并进行了手性色谱拆分评价。与单侧链取代的刷型固定相进行对比,C_2对称型手性固定相对所评价的31种酸性、中性和碱性分析物表现出更好的手性选择性。考察了固定相末端苯环上的取代基团对手性拆分的影响,综合来看,苯环上无取代基的C_2对称型手性固定相的分离性能最优。对某些手性对映体,C_2对称型手性固定相的分离因子随温度的增高而呈现异常增大的现象,表明了其有别于单侧链取代的固定相的分离机理。该类新型手性固定相的提出对进一步丰富刷型手性固定相的种类和拓展其应用具有重要意义。     

EQUILIBRIUM MODELING OF PSEUDOMONAD AGGREGATION AND PARTITIONING TO DOLOMITE†

Bioremediation is a common treatment technology considered for the remediation of many toxic and hazardous waste sites. In order for this technology to be successfully implemented, the mobility and adhesion characteristics of the microorganisms must be understood. This study explored the surface and adhesion characteristics of two pseudomonads: Pseudomonas aeruginosa Olin and P. fluorescens rib:lux. In general, the Lewis acid/base character of these microorganisms dominated surface thermodynamics. In both cases partitioning to dolomite, a common mineral, was predicted to be greatest in the stationary phase. In the log growth and decay phases, the Lewis acid/base interaction energy was repulsive for both organisms. The stationary phase for both microbes exhibited a reversal of the Lewis acid/base energy to attractive. Although the magnitude of the various surface energy components differed between the microorganism, it is remarkable that the Lewis acid/base energy exhibited similar behavior.     

LC and LC-MS Separation of Peptides on Macrocyclic Glycopeptide Stationary Phases: Diastereomeric Series and Large Peptides

Previous work on the LC separation of peptides had shown that macrocyclic glycopeptide stationary phases to be selective for peptides of five to thirteen amino acids in length. In this work, the selectivity of the teicoplanin stationary phase is compared to that of a C18 stationary phase for seven diastereomeric enkephalin peptides. The teicoplanin stationary phase separated all seven diastereomeric enkephalin peptides in a single chromatographic run. The insertion of d-amino acids into the primary enkephalin sequence produced areas of hydrophobicity that influenced retention order on the C18 stationary phase. However, analogous trends are not observed on the teicoplanin stationary phase, which is more polar and structurally diverse. Optimization of the mobile phase and the use of a step-gradient for the enkephalin separation on the teicoplanin stationary phase is discussed. Also, the selectivity of macrocyclic glycopeptide stationary phases for peptides of 14, 28, 30, and 36 amino acids also is investigated and compared to separation on a C18 stationary phase. A method for eluting peptides with multiple basic amino acids, which tend to be strongly retained on the macrocyclic glycopeptide stationary phases, is presented.     

Retention behavior of basic compounds on alkylphosphonate-modified magnesia-zirconia composite stationary phase in RPHPLC

Summary The chromatographic properties of an alkylphosphonate-modified magnesia-zirconia composite stationary phase have been investigated by reversed-phase high-performance liquid chromatography with basic compounds as probes. The influence of organic modifier composition and mobile phase pH was studied. The new stationary phase, similar to a silica-based reversed-phase stationary phase, has hydrophobic properties, but greater pH stability. Use of the phase results in more symmetric peaks for basic compounds. A possible mechanism of retention of basic solutes on the new stationary phase is discussed. The chromatographic behavior of the basic solutes depends mainly on hydrophobic interactions between the solutes and the hydrophobic moiety of the stationary phase. Br?nsted acidic and basic sites on the surface of the new stationary phase play an important role in the retention of ionized solutes by ion-exchange interaction. Promising separations of some basic compounds have been achieved by use of methanolic TRIS buffer, pH 10.0, as the mobile phase.     

High-Performance Liquid Chromatography of some Bases and Nucleosides on Alkylphosphonate-Modified Magnesia-Zirconia Column

ABSTRACT

The high-performance liquid chromatographic behavior of some bases and nucleosides was studied on a new reversed-phase stationary phase, alkylphosphonate-modified magnesia-zirconia. The effect of mobile phase variable such as methanol content, ionic strength and pH on their behavior was investigated. It was found that the retention behavior of the bases and nucleosides on the new stationary phase is similar to that on ODS stationary phase. The retention mechanism on the new stationary phase was also discussed. The separation of some bases and nucleosides was accomplished on the new stationary phase.     

咪唑侧基功能化聚离子液体修饰的混合模式色谱固定相的制备及其色谱性能

该文合成了咪唑侧基功能化的离子液体单体1-(4-乙烯基苄基)-3-氰甲基溴化咪唑盐,通过表面引发原子转移自由基聚合将该单体接枝到硅胶表面,制备了一种新型混合模式色谱固定相。采用红外光谱、元素分析及热重分析对其结构进行表征。该色谱固定相具有良好的分离能力。通过研究流动相pH对物质保留的影响,验证了物质在该固定相上存在反相-离子交换保留机理。通过与十八烷基硅烷键合硅胶固定相比较,证实了该聚离子液体固定相对物质保留提供了π-π作用。结果表明,对咪唑侧基功能化是制备新型离子液体固定相的可行方法。