巯基键合银离子色谱固定相的制备及其 在油脂分析中的应用

目的建立一种巯基键合银离子色谱固定相的制备方法。方法以活化硅胶为原料,巯丙基三甲氧基硅烷为偶联剂,在邻二甲苯溶液中合成巯丙基键合硅胶,利用巯基与银离子之间的键合作用合成银离子色谱固定相。采用红外光谱、元素分析与银离子负载量对其进行表征,以0.5%乙腈-正己烷(V:V)溶液为流动相,对5种不同不饱和脂肪酸标样及4种常见食用油中的不饱和脂肪酸甲酯进行分离分析与评价。结果经表征与分析可知,巯丙基硅胶键合银离子效果很好,其银离子负载量为0.182 g/g,该分析条件下,对于常见不饱和脂肪酸甲酯的具有很好分离效果,且具有很好的稳定性与重现性。结论该巯基键合银离子色谱固定相对不饱和脂肪酸甲酯具有较好的分离能力,在多不饱和脂肪酸的分析、分离纯化方面具有较好的应用潜力。     

液相色谱在食品检测中的应用

液相色谱技术是一种高效的分离和分析技术,其流动相为液体,固定相有纸、填充床、薄板等多种形式。液相色谱技术在食品检测中的应用十分广泛,本文从液相色谱的原理入手,浅谈了液相色谱在食品检测中应用。     

三聚氰胺固定银离子色谱固定相的制备及其在油脂检测中的应用

以异氰酸丙基三乙氧基硅烷为偶联剂,三聚氰胺为配体,制备了三聚氰胺键合硅胶色谱固定相,利用三聚氰胺和银离子的络合作用,进一步合成得到三聚氰胺固定银离子色谱固定相。采用红外光谱和元素分析对其进行表征,测得三聚氰胺键合量为0.11 mmol/g,通过分光光度法测得银离子负载量为0.17 g/g。在洗脱体系为乙腈-正己烷(体积比0.3∶99.7)、流速0.5 m L/min条件下,该银离子色谱柱对5种不饱和脂肪酸甲酯混合标样完美分离,应用于4种常见油脂样品中不饱和脂肪酸的测定中亦获得较好效果。     

高效液相色谱技术在食品检测中的应用

高效液相色谱法是化学分离分析的一种重要手段和技术,应用比较广泛。本文研究高效液相色谱技术在食品检测中的具体应用,综述了食品中的糖类、氨基酸类、维生素类、食品添加剂、有毒食品等成分分析中高效液相色谱法的应用方向。     

高速逆流色谱及其在天然产物分离中的研究进展

高速逆流色谱（high speed countercurrent chromatography,简称HSCCC）是一种快速、高效、连续的液-液分配色谱分离技术,在中药、生化、食品、天然产物化学、环境分析等领域有着广泛的应用。本文对高速逆流色谱技术及其在天然产物功能性成分分离中的应用进行了综述。      

柑橘活性成分检测技术研究进展

柑橘中富含类黄酮、类柠檬苦素、类胡萝卜素、酚酸等多种生理活性成分,在功能食品和药品开发方面具有广阔的应用前景。文中综述了近年来柑橘中主要活性成分的分离及检测技术进展,着重介绍了高效液相色谱在柑橘活性成分检测中的应用。     

现代色谱技术在天然产物研究中的应用

天然产物来源广泛、种类繁多、结构复杂且多数未知。随着人们对天然产物认识的深入以及仪器分析检测技术的进步，天然产物的开发与利用日益受到重视。近年来发展的新型色谱模式、色谱-质谱联用、谱效关联等现代色谱技术不但促进了天然产物的分离检测与纯化制备，同时推动了天然产物活性物质的阐明，加快了天然产物研究的步伐。基于上述现代色谱技术，本文结合文献主要从分析检测、分离制备、活性筛选这3个层面综述其在天然产物活性物质研究方面的应用，以期为进一步发展色谱技术在天然产物的开发与利用中提供一定的参考依据，希望通过本文的研究可以促进色谱技术在天然产物活性成分提取与纯化领域的快速发展。     

模拟移动床技术在天然产物分离制备中的应用

随着模拟移动床色谱技术(simulated moving bed,SMB)的快速发展,该技术在天然产物活性成分的提取与纯化中的应用日益广泛。本文简述了SMB技术的发展和在天然产物分离中的应用现状,并重点介绍了SMB技术在黄酮类、多酚类、氨基酸以及肽类和糖类分离制备中的应用。与传统的制备色谱技术相比,SMB采用连续操作手段,具有易于自动化操作、制备效率高、制备量大等特点,在天然产物分离制备中具有良好的发展前景。     

山茱萸中具有抗氧化活性的环烯醚萜类成分

采用正相硅胶柱色谱、Sephadex LH-20凝胶柱色谱、大孔吸附树脂柱色谱、氰基柱色谱和高效液相色谱等方法对山茱萸乙醇提取物中具有抗氧化活性的环烯醚萜类组分进行分离纯化;采用核磁共振波谱技术和质谱技术鉴定其结构;通过总抗氧化能力FRAP法测定其抗氧化活性。结果表明：共分离并鉴定出4个具有抗氧化活性的环烯醚萜类成分,分别为：马钱子苷（1）、马钱素-7-酮（2）、1-β-甲氧基马钱子苷元（3）和1-去羟基马钱子苷元（4）,其中化合物3和4是首次从山茱萸属中分离得到的新的天然产物。     

吡唑醚菌酯残留分析研究进展

吡唑醚菌酯是一种新型甲氧基丙烯酸酯类杀菌剂,广泛用于防治水果、蔬菜、谷物等作物中的白粉病、锈病、网斑病、霜霉病、稻瘟病等病害。本文对吡唑醚菌酯的残留分析方法进行了综述。在样品前处理中,以octadecyl silica(C18)、N-丙基乙二胺或石墨化碳黑为填料的固相萃取技术应用最为广泛;涂装聚二甲基硅氧烷、二乙烯基苯等的固相微萃取技术,由于具有很高的灵敏度近年来也已大量应用;基质固相分散、凝胶渗透色谱、分散固相萃取等技术的应用,使净化效率大大提高。在样品分析中,传统的气相色谱、高效液相色谱特别是后者虽然仍在大量应用,但气相色谱-串联质谱、高效液相色谱-串联质谱技术由于具有极高的选择性和灵敏性,已得到迅速发展和广泛应用。酶联免疫吸附分析、胶束电动毛细管色谱、近红外光谱技术等分析检测技术的应用潜力很大。     

高效液相色谱法快速鉴别人工合成虾青素养殖的三文鱼

建立了虾青素手性异构体分离和检测的HPLC 方法。条件：采用手性固定相色谱柱;Pirkle L- 亮胺酸(4.6mm × 25cm,5μm); 流动相：正己烷- 四氢呋喃- 异丙醇- 三乙胺(77:17:3:3,V/V);紫外检测波长：474nm;流速：0.75ml/min。本法可应用于快速鉴别养殖三文鱼是否使用了人工合成虾青素,并可以初步判断是否为野生三文鱼。     

软枣猕猴桃根中蒽醌类化合物的分离纯化和含量测定

利用聚酰胺柱层析和硅胶柱层析法从软枣猕猴桃根中分离纯化蒽醌化合物,采用高效液相色谱法分析法检测软枣猕猴桃根中蒽醌类化合物的含量。结果表明：分离的最佳条件为200 目硅胶、φ1.1 cm×100 cm层析柱、洗脱剂流速1.5 mL/min;甲醇-水（90∶10,V/V）流动相、254 nm检测波长的高效液相色谱测定软枣猕猴桃根中蒽醌主要组分为大黄素和大黄酚,其含量分别为46 μg/g和157.5 μg/g。     

肽类生物表面活性剂中消泡剂的分离研究

本研究首次建立硅胶柱层析两步法以去除抗菌脂肽粗品中所含有的大豆油消泡剂成分,实验中采用高效液相色谱（HPLC）检测抗菌脂肽的含量,薄层色谱-可见光分光光度法定量分析消泡剂中甘油三酯含量,TLC法筛选大豆油的洗脱流动相。研究结果表明:使用200³00目的硅胶作为层析材料,硅胶的总负载量为12.5mg/g时,采取混合液（石油醚∶乙酸乙酯∶乙酸=20∶2∶1,体积比）为流动相,以1m L/min流速进行洗脱,可将97.97%的大豆油成分去除;第二阶段采用流动相为100%的乙醇以1m L/min流速进行洗脱可将抗菌脂肽解吸,抗菌脂肽的总回收率达到91.52%,纯度从34.07%提高到93.12%。本研究为肽类生物表面活性剂工业化生产和应用提供实验依据。      

Identification des filtres UV dans les produits cosmétiques par CCM et HPLC

The method describes the identification of 22 UV filters authorized in Cosmetic products in Europe (dir. 76/768 EEC, annex VII, modified by dir. 89/174 EEC). (Table I).
Twelve UV filters registered in part 2 of annex VII (dir. 83/574EEC) provisionally allowed in 1983 were abandoned by Industry. Consequently they were suppressed from the list of UV filters which cosmetic products may contain (dir. 89/174 EEC). Nevertheless the method describes also the identification of these 12 chemicals because they could interfere with the analysis of the 22 authorized UV filters in view of similarities in chemical structures (Table I (suite)).
The screening of the UV filters in final products is based on thin layer chromatography (TLC) and confirmed by high pressure liquid chromatography (HPLC/UV).
TLC combines four different systems and several detection reagents: absorption chromatography on silica gel with development in a neutral solvent, an acidic solvent, a basic solvent, reversed phase chromatography on RP 18 bonded silica with development in a methanol/water mixture.
The results of these screening tests are confirmed by reversed phase HPLC/UV in an isocratic elution system. The acid components and the salts which are eluted before or with the solvent peak are separated in a gradient elution system at pH 3.5.
Several UV filters available on the market of cosmetic ingredients are impure chemicals or mixtures.
The identification of their principal components by nuclear magnetic resonance spectrometry (NMR) and by gas chromatography/mass spectrometry (GC/MS) will be the subject of future publications.     

Some analytical aspects of enzyme degradation of starch and inulin into malto- and fructooligosaccharides

The determination of some quantitative parameters of starch hydrolysis, as well as the determination of some analytical properties during vegetation period and storage of Jerusalem artichoke and hydrolysis of inulin are of great importance for conducting the integrated technological process. The consequences which result from this are very important. High performance liquid chromatography (HPLC) has been used in order to solve these very complex analytical problems. Stationary phase ZORBAX-NH₂, aminomodified silica dioxide. has been used successfully for chromatographic determination of the given substrates. This HPLC procedure has some greater advantages over the procedures which have been used up to now for this purpose.     

果蔬中常用植物生长调节剂分析方法研究进展

近年来,植物生长调节剂在果蔬生产中的使用越来越多,随着人们对其残留危害的日益关注,痕量植物生长调节剂残留的分析技术也在不断发展。文中概述了国内外检测果蔬中植物生长调节剂残留的主要分析方法及其优缺点,包括气相色谱(GC)、高效液相色谱(HPLC)、质谱联用技术、酶联免疫吸附测定(ELISA)、毛细管电泳(CE)及其他分析法,并对其发展趋势进行了展望。     

Application of reversed phase liquid chromatography in the analysis of saponins in faba bean

Due to the high biological activity of saponins this group of compounds has become the object of interest of many researchers from different scientific disciplines [7]. In the analysis of saponins the stage of isolation of an investigated compound which follows the extraction from the plant material is decisive. Liquid column chromatography, e.g. ion-exchange chromatography [12], silica gelchromatography [1, 4, 5, 11], gel filtration on Sephadex LH-20 [6, 9, 10] and reversed phase chromatography have been used in the procedure. In the case of the latter columns were filled with octasilane [8] or octadecylsilane (ODS) bonded to silica gel [2, 4, 11]. The aim of the study was to apply reversed phase liquid chromatography in the analysis of saponins in faba bean.     

A comparison of the TLC-densitometry and HPLC method for the determination of biogenic amines in fish and fishery products

A comparative study on the suitability of chromatographic techniques such as thin layer chromatography (TLC)-densitometry and high performance liquid chromatography (HPLC) for the analysis of biogenic amines in fish and fishery products was carried out. The HPLC method was found to offer a good linearity (5–100 ng), sensitivity and repeatability (<3%), but required sophisticated instrumentation, technical skill and high operational cost and time. On the other hand, with a little loss in linearity (20–300 ng) and repeatability (<8%), TLC-densitometry was found to be rapid and less expensive. In addition, this method is suitable for rapid and simultaneous screening of several samples at a time. Therefore, the TLC-densitometric method can be effectively used in the fish industry to detect biogenic amines, especially the toxic histamine, and putrescine and cadaverine, which can potentiate histamine toxicity in fish and fishery products.     

Analyses of Glycolipids in Clove, Red Pepper, and Nutmeg by High-Performance Liquid Chromatography

ABSTRACT: To determine the existence of glycolipids (neutral glycosphingolipid and glycoglycerolipid) in clove, red pepper, and nutmeg, we performed silica gel chromatography and high-performance liquid chromatography (HPLC) using an Aquasil-SS column and a C₈-reversed-phase silica gel column. HPLC (Aquasil-SS column) with a UV absorption detector was used to analyze neutral glycosphingolipid. These chromatograms showed two typical peaks in clove lipids. UV-HPLC (C₈-reversed phase silica gel column) was also used to analyze glycoglycerolipid. The chromatograms indicated a small peak in clove lipids. Moreover, we observed the same two peaks in the glycolipid fraction of clove lipid when we used HPLC (Aquasil-SS column) with a differential refractometer detector. These results suggest that clove may contain new and plural neutral glycosphingolipids.     

METHYL DIHYDROJASMONATE AND ITS STEREOISOMERS: SENSORY PROPERTIES AND ENANTIOSELECTIVE ANALYSIS

Enantiomeric methyl dihydrojasmonates (MDHJs) were separated by chiral gas chromatography (GC) and high performance liquid chromatography. Organoleptical evaluation clearly revealed that all four stereoisomers are odor-active and differ in their olfactory properties. Using enantio-multidimensional capillary GC-mass spectrometry with heptakis(2,3-di-O-methyl-6-O-tertbutyldimethylsilyl)-β-cyclodextrin as the chiral stationary phase, the direct enantioselective analysis of all four stereoisomers of MDHJ in numerous natural products was achieved for the first time.