Investigation of separation and identification possibilities of some metal-DEDTC complexes by sequential TLC-IR system

The separation and identification possibilities of some metal-diethyldithiocarbamate (DEDTC) complexes are investigated by thin-layer chromatography-IR sequential system. DEDTC complexes of metal cations are prepared in a predetermined optimum pH or pH range. Optimum separation conditions of these complexes and the reproducibilities of their retention factor (Rf) values are investigated on a series of precoated or laboratory-made TLC plates. Rf values are determined using the one-dimensional ascending technique. The precision of the procedures is determined for five replicates in terms of standard deviation. Detection limits are also determined for each of the metal complexes. The IR spectra are scanned and interpreted for their precise identifications after preconcentration with a wick-stick procedure for the complexes, giving the overlapped Rf values. The complexes could be identified by the aid of IR absorption bands. It has been determined that these IR absorption bands can also be used as reference spectral bands in possible quantitative studies. It is concluded that an efficient and successful qualitative analysis is possible for incompletely-separated complex compounds using an IR spectrophotometer as the TLC detector.     

Separation and Identification of Microplastics in Digestive System of Bivalves

A pretreatment method was established for separating microplastics from digestive system of bivalve sample. Qualitative and quantitative analysis of microplastics was carried out by micro-Fourier transformed infrared (μ-FT-IR) spectroscope and Stereo microscope. The method was applied to analyze the microplastics in the digestive system in Chlamys farreri and Mytilus galloprovincialis. The results showed that the digestion system of using 10% KOH had high digestion efficiency. With this digestion system, the recoveries of polypropylene (PP), polyethylene (PE), polystyrene (PS) and polyvinyl chloride (PVC) ranged from 96.7% to 98.6%, with relative standard deviation (RSD, n = 3) of ≤ 3.19%. We collected Chlamys farreri from local markets (n = 50) and Mytilus galloprovincialis from both local markets (n = 50) and wild environments (n = 15) in Qingdao, China. The results showed that microplastics were found in over 80% of the individuals purchased from the market and 40% of the wild collected individuals. The average abundance of microplastics in Chlamys farreri purchased from different markets varied between 5.2 and 19.4 items/individual or between 3.2 and 7.1 items g^?1 (wet weight of digestive system), while in Mytilus galloprovincialis, the numbers varied between 1.9 and 9.6 items/individual or between 2.0 and 12.8 items g^?1. Farmed mussels (Mytilus galloprovincialis) contained more microplastics (average 1.9 items per individual, 3.17 items g^?1) than wild mussels (average 0.53 items individual, 2.0 items g^?1). Three shapes of microplastics, including fibers, fragments and granules were separated from the samples above. Among which, fibrous microplastics, being the most dominant ones, took up 84.11% of total microplastics. The average size of fibrous microplastics ((0.66 ± 0.70) mm) was larger than that of the other two shapes of microplastics. The number of microplastics decreased with increasing microplastic sizes. Microplastics of less than 500 μm coming from different markets were in the range of 26% to 84%. And it was found that the most common polymer component in the samples was cellophane (CP), followed by polypropylene (PP). The method has some advantages such as simplicity, high efficiency, and low damage to the microplastics in the sample, and can be used to detect and analyze microplastics in seafood.     

Separation and Identification of Labile Polyacetylenes by RP-HPLC

Abstract

Traditional methods of isolation and identification of labile polyacetylenes often lead to substantial loss of material. Reverse-phase HPLC coupled with a diode array detector offers a fast and convenient way to isolate and identify polyacetylenes from plant sources. Minimizing the number of manipulations reduces the potential for losses, and makes a more accurate quantitative analysis of the polyacetylenes possible.     

用毛细管电泳法对某些药物的分离试验

本文采用毛细管电泳法,以50μm内径,45cm长的弹性石英毛细管作为分离管,选用磷酸盐-硼酸盐-十二烷基硫酸钠缓冲溶液体系,在柱254nm紫外检测器,在不同的电泳电压下,对水溶性维生素,磺胺类药物、头孢菌素抗生素,解热镇痛药物有效成份进行了分析,取得较满意的结果。     

EDTA金属螯合物阴离子交换色谱行为研究

本文报道Ｚｎ（Ⅱ）、Ｃｒ（Ⅲ）、Ｆｅ（Ⅲ）等金属－ＥＤＴＡ螯合物的阴离子交换色谱行为．采用ＰＲＰ－１００阴离子色谱柱，以２．０ｍＬ／ｍｉｎ．流速、４ｍｍｏｌ／Ｌ苯甲酸为淋洗液，电导检测器检测，可以很好地分离Ｚｎ－ＥＤＴＡ２－、Ｃｒ－ＥＤＴＡ－、Ｆｅ－ＥＤＴＡ－．方法可用于废水中金属离子的检测．     

Low-Pressure Chromatographic Separation of p-Hydroxybenzoates Using Sequential Injection with Lab-on-Valve System and Miniature Monolithic Column

The use of a small guard column (5-mm length) as a miniature analytical column in low-pressure liquid chromatography based on a sequential injection with lab-on-valve system was demonstrated. A strong initial mobile phase was used to rapidly deliver the sample zone to the column prior to simultaneous separation of analytes with weaker mobile phase. Separation of methyl-, ethyl-, propyl-, and butyl-4-hydroxybenzoates (MP, EP, PP, and BP) was achieved within about 120 s with sufficient peak resolution (all higher than 1.3) using 2,500 µL of mobile phase (composed of 1,087 µL of MeOH) per run. Detection limits were found to be 6.5, 8.0, 0.5, and 0.6 μmol L^?1 for MP, EP, PP, and BP, respectively. The system was tested with common commercially available skin lotions and wet wipe products. The analysis results were in good agreement with those obtained from the high-performance liquid chromatography with a 10-cm-length packed column.     

生物小分子钒配合物抑制蛋白酪氨酸磷酸酶活性研究

钒化合物治疗糖尿病机理研究表明其与蛋白酪氨酸磷酸酶的酶活抑制有一定关系。本文分别研究了生物小分子配体与氧钒离子在20:1配比条件下形成的生物小分子钒配合物及其对蛋白酪氨酸磷酸酶的抑制作用和选择性。结果表明氨基酸与氧钒离子配合形成2:1的配合物,而抗坏血酸及多羧酸与氧钒离子配合形成1:1的配合物。它们对蛋白酪氨酸磷酸酶抑制作用显示,大部分生物小分子氧钒配合物对PTP1B表现强烈的抑制作用,IC50值在0.12~0.63μmol.L-1之间。化合物[VO(Phe)2]表现最强的抑制作用,IC50值为0.07μmol.L-1。而[VO(Arg)2]、[VO(Oxalate)]、[VO(Nitrilotriacetate)]和[VO(Citrate)]则呈现较弱的抑制,IC50值分别为1.05、1.41、9.90和21.5μmol.L-1。对PTP1B,TCPTP,HePTP以及SHP-1的抑制作用表明配体的结构不仅影响氧钒配合物对蛋白酪氨酸磷酸酶的抑制效率同时也影响其选择性。     

生物小分子钒配合物抑制蛋白酪氨酸磷酸酶活性研究

钒化合物治疗糖尿病机理研究表明其与蛋白酪氨酸磷酸酶的酶活抑制有一定关系。本文分别研究了生物小分子配体与氧钒离子在20:1配比条件下形成的生物小分子钒配合物及其对蛋白酪氨酸磷酸酶的抑制作用和选择性。结果表明氨基酸与氧钒离子配合形成2:1的配合物, 而抗坏血酸及多羧酸与氧钒离子配合形成1:1的配合物。它们对蛋白酪氨酸磷酸酶抑制作用显示, 大部分生物小分子氧钒配合物对PTP1B表现强烈的抑制作用, IC₅₀值在0.12~0.63 μmol·L^-1之间。化合物[VO(Phe)₂]表现最强的抑制作用, IC₅₀值为0.07 μmol·L^-1。而[VO(Arg)₂]、[VO(Oxalate)]、[VO(Nitrilotriacetate)]和[VO(Citrate)]则呈现较弱的抑制, IC₅₀值分别为1.05、1.41、9.90和21.5 μmol·L^-1。对PTP1B, TCPTP, HePTP以及SHP-1的抑制作用表明配体的结构不仅影响氧钒配合物对蛋白酪氨酸磷酸酶的抑制效率同时也影响其选择性。     

顺序注射-液芯波导-激光诱导荧光微流控电泳系统分析脱氧核糖核酸

报道了一种基于液芯波导的小型激光诱导荧光微流控分析系统及其在分离检测DNA样品中的应用。使用6 cm长Teflon AF涂覆的石英毛细管作为液芯波导管,同时作为电泳分离通道和荧光检测光路,将分离后样品的荧光信号传送到检测器。半导体激光器(LD)作为激发光源,产生的荧光信号在波导管出口收集。设计了一种特殊的出口储液池,直接使用滤光片作为液池的后壁并置于光电倍增管(PMT)窗口处,从而使全部检测系统仅由LD、LCW、滤光片和PMT四部件组成,达到了结构最简化。使用顺序注射(SI)系统实现了自动样品更新,该系统通过一种改进结构的可消除气泡的接口与微流控系统联接。采用这种联用系统实现了溴化乙锭(EB)标记的X174-HaeⅢ裂解液中11个脱氧核糖核酸片段的分离和聚合酶链反应扩增样品的检测。     

Separation and Identification of Glycosaminoglycans

The term “mucopolysaccharides” was originally introduced by Meyer to describe “hexosamine-containing heteropolysaccharides of animal origin occurring in a pure state or as protein salts”. Many of the names originally assigned to the mucopolysaccharides have since been revised in an effort to systematize the nomenclature (Table 1). Jeanloz² in 1960 proposed the term “glycosaminoglycuronoglycans” in place of mucopolysaccharides as in most cases they are composed of amino sugars (glycosamino-) and uronic acids (glycurono-) joined in long chains(-glycans). For the sake of simplicity, the term “glycosaminoglycans” is getting acceptance in place of the rather lengthy term “glycosaminoglycuronoglycans” as well as the old and perhaps more familiar term “mucopolysaccharides”. As a matter of convenience, the term “polysaccharides” will be frequently used here, instead of glycosaminoglycans.     

Isoselective Polymerization of rac-Lactide by Highly Active Sequential {ONNN} Magnesium Complexes

The coordination chemistry and the activities in the ring-opening polymerization catalysis of racemic lactide (LA) of magnesium complexes of a series of {ONNN}-type sequential monoanionic ligands are described. All ligands include pyridyl and substituted-phenolate as peripheral groups. The ligands bearing either chiral or meso-bipyrrolidine cores led to single diastereomeric complexes, whereas the ligands bearing a diaminoethane core led to diastereomer mixtures. All {ONNN}Mg-X complexes [X=Cl, HMDS (hexamethyldisilazide)] led to highly active and isoselective catalysts. The complexes bearing the chiral bipyrrolidine core exhibited the highest activities (full consumption of 5000 equiv. of rac-LA at RT within 5 min) and highest isoselectivities (P_m=0.91), as well as a living character. The complexes of the meso-bipyrrolidine based ligands were almost as active and slightly less stereoselective, while those of the diaminoethane based ligands exhibited reduced activities and isoselectivities.     

Sequential Separation and Indirect Voltammetric Determination of Silicate and Phosphate

Abstract

An indirect voltammetric method for the determination of silicate at the ppm level was developed. The method is based or. the D.C. polarographic current measurement of molybdate ion formed by the decomposition of 12-molybdophosphoric and 12-molybdosilicic acids. After separation of the heteropoly acids by the liquid-liquid extraction technique, the heteropoly acids are decomposed with a basic buffer. After adjusting the solution to the proper conditions, the current measurement is made at the dropping mercury electrode.     

Identification and Separation of Some Anions on Plain and Mixed Adsorbent Layers Using Water as Eluent

The analytical potential of water as an eluent in thin layer chromatographic separation of various anions on plain adsorbent layers (silica gel "G" alumina, and cellulose) as well as on beds containing different combinations of silica gel, alumina, or cellulose has been investigated. In addition to some important separation of anions, microgram separation of IO⁻₄ from milligram quantities of IO⁻₃, Bro⁻₃, MoO²⁻₄, and Fe (CN)³⁻₆ has been realized. The effect on pH of the sample in the separation of IO⁻₄ from accompanying ions has also been studied. The limits of detection and dilution limits of anions on alumina thin layers have been determined. NO⁻₂ in artificial seawater has been detected. The effect of CaCl₂, MgCl₂, and NaHCO₃ on some ternary separations of analytical importance has been examined.     

金属硫蛋白异构体及亚型异构体的液相色谱分离与质谱鉴别

建立了金属硫蛋白(MT)异构体及亚型异构体的色谱分离与质谱鉴别方法。将金属硫蛋白混合物通过弱阴离子DEAE Sephadex A-25离子交换柱,结合离线电感耦合等离子体质谱(ICP-MS)对锌诱导金属硫蛋白的两个异构体MT-1和MT-2进行分离和检测;利用Sephadex G-25凝胶排阻色谱柱对得到的两个金属硫蛋白异构体进行脱盐;探索脱盐后的金属硫蛋白异构体在不同色谱条件下的C18反相色谱柱上的保留行为,进而实现各个亚型异构体的分离;通过在线电喷雾质谱检测实现了对金属硫蛋白各个亚型异构体的鉴别。结果表明,通过优化色谱条件,由离子交换色谱及凝胶排阻色谱得到的金属硫蛋白各亚型异构体在酸性条件下均得到了良好的分离,质谱检测结果与前人的文献报道结果一致。该方法可使金属硫蛋白各异构体均达到最佳的分离效果。     

稀土—5—Br—PADAP螯合物的高效液相色谱分离与测定

以配合物形式分离金属离子已有报道.胡之德等研究了In、Pt、Pd等金属与5-Br-PADAP螯合物的色谱行为,在硅胶柱上成功地分离了这几种金属元素.林长山等应用反相高效液相色谱法,分离了Fe(Ⅲ)、Co(Ⅱ)和V(Ⅱ)3种金属的5-Br-PADAP螯合物,并做了定量的研究.本文应用高效液相色谱法研究了镧系-5-Br-PADAP螯合物色谱行为,探讨了相关因素对分离和测定的影响,讨论了螯合物的保留值与稀土元素原子半径的关系.     

Electrochromatographic Separation of DMSO Complexes of Metal Ions

Abstract

Electrochromatography of DMSO complexes of fourteen metal ions have been performed in five electrolytes at 100 volts for 3 hrs. The mechanism of migration has been explained and a number of separations of metal-DMSO complexes were achieved.     

反相高效液相色谱对DABTH—氨基酸的分离与鉴定

应用反相高效液相色谱(RP-HPLC)技术,采用等度洗脱。对20种标准DABTH-氨基酸进行了分离与鉴定,灵敏度达到pmol水平;并以溶菌酶为模式蛋白,经手工DABITC/PITC双偶联方法对其N端部分序列进行Edman降解,其降解产物DABTH-氨基酸用RP-HPLC技术进行了鉴定,蛋白质微量序列分析的灵敏度达到nmol水平.