发表咨询:400-808-1731
订阅咨询:400-808-1751
摘要:A typical analytical separation procedure has several important steps: sample preparation, isolation, identification, quantitation, statistical evaluation and final decision. Each step is always critical to obtain correct results to fulfill the analytical purpose. In these various steps sample preparation step is required in order to isolate the desired components from some sample matrix since most instruments cannot handle the matrix directly and also it should include "clean up" procedure for complex dirty samples. This step needs to bring the analytes to a suitable concentration level that can be measured by the method for the real instrumental analysis, and this is called as "preconcentration" step. As the next step the isolation includes various chromatographic separation methods that the most appropriate one can be chosen depending on the analytes properties, for example, volatile and thermally stable compounds can be analyzed by gas chromatography (GC), and non-volatile and thermally labile compounds should be analyzed by liquid phase separations such as liquid chromatography (LC) and capillary based electrodriven techniques like capillary electrophoresis (CE) and capillary electrochromatography (CEC). By these analytical separation techniques the isolated complex mixture containing target analytes can be separated into its constituents. Identification and quantitation can be performed by a retention information combined with selective detection such as mass spectrometer (MS) to eliminate the interferences. Two additional steps can be done recently by using some computer techniques so-called chemometrix methods.
摘要:The separation and identification of complex samples is an urgent task that analytical chemistry has to face. Chromatography, as an important analysis technique, has been widely applied to many fields, such as life science, environment, medicine, food and petrochemical engineering. Recently, with the progress of science and technology, higher and higher requirements have been put forward for the analysis of practical samples. Accordingly, chromatography has simultaneously undergone rapid development. Here we would like to make a brief summary on the newest research results of National Chromatographic R. & A. Center, and hopefully it could reflect the advances of chromatography in the analysis of complex samples.
摘要:Molecular recognition plays an important role in biological and chemical processes. Since molecular imprinting techniques can afford complementary binding sites for a target molecule, the molecularly imprinted polymer (MIP) for the target molecule has been used for its specific recognition as chromatographic media, solid-phase extraction media, artificial antibodies, membranes and sensors[1-4]. Usually, MIPs were prepared by a bulk polymerization method. However, the disadvantage of the method is that the obtained block polymers should be crushed, ground and sieved to produce high performance liquid chromatographic (HPLC) packing materials. Recently, we prepared the uniformly sized MIPs by a multi-step swelling and polymerization method[5], which is suitable for preparing HPLC packing materials, and renders in situ modification susceptible.
摘要:The separation of enantiomers is of great importance in biology, pharmaceutics, agriculture and environment. The different separation modes (i.e. capillary zone electrophoresis (CZE), micellar electrokinetic chromatography (MEKC), capillary electrochromatography (CEC), etc) and many chiral selectors available make capillary electrophoresis (CE) technique a powerful tool for chiral analysis[1]. On the basis of ligand-exchange (LE) mechanism introduced by Davankov and Rogozhin[2] in the early 1970s for high performance liquid chromatography (HPLC), the first application of CE in chiral separation was reported by Zare's group[3,4]. Using Cu(Ⅱ) complexes of L-histidine or aspartame as chiral selectors, 14 dansyl amino acids (Dns-AAs) were resolved. The authors observed a significant improvement in resolution when a micelle forming surfactant such as sodium dodecyl sulfate (SDS) was added to the electrolyte performing MEKC. The method was called as ligand-exchange micellar electrokinetic capillary chromatography (LE-MEKC). As a hybrid mode of possessing both the advantage of high enantioselectivity in ligand-exchange mechanism and the main advantages of MEKC, LE-MEKC allows the manipulation of the selectivity for large classes of neutral and charged compounds, making possible separation that otherwise are not feasible by using only the mode of LE or MEKC. Using this combined separation mode, hydroxy acids and dipeptides, as well as 16 positional and optical isomers of tryptophan derivatives could be optically resolved[5]. The same group also proposed a method for the determination of the critical micelle concentration (CMC) of anionic surfactants based on LE-MEKC principle[6].
摘要:The flow diagram of this on-line sample pretreatment system is shown in Fig.1.
摘要:As an important constituent in the biomembranes, phospholipids (PL) are a complex mixture of molecular species containing a variety of fatty acyl and head group compositions. In addition to their structural role, some phospholipids also participate in biological processes in various ways, such as cellular signaling[1]. Phospholipids have received increased attention in many fields, for example as biomarkers in chemotaxonomical studies and in the making of liposomes for drug delivery or cosmetics/detergents.
摘要:1 Introduction Since human genome sequencing has been almost completed, human genome project will quickly move on to the post genome sequencing era, including single nucleotide polymorphism (SNP) analysis, functional genomics, mutation analysis, transcriptome analysis, proteome analysis, and metabolome analysis[1,2]. Capillary array electrophoresis with 96-384 capillaries plays a vital role in the genome sequencing era, but in the post human genome sequencing era, further development of analytical technology for deoxyribonucleic acid (DNA), messenger ribonucleic acid (mRNA), protein, and metabolites is highly required for future medicine and new drug discovery technology based on functional genomics and proteomics[3-13].
摘要:Capillary electrophoresis (CE) has rapidly gained great interests among researchers in many different fields. One of these areas is the separation of small ions such as inorganic cations[1-9], anions[10-16], and low Mr organic molecules[17-20]. However, as the separation of ions by CE is depended on the difference in electrophoretic mobilities of the ions, and this difference for some of them are very small. Thus, a background electrolyte (BGE) system must be selected to modify the mobilities of the analyte ions, e.g., the actual mobilities of some alkali, alkaline earth metal and ammonium cations are very similar[21].
摘要:In recent years, the synthesis of chiral tetrahedral clusters has been studied extensively and various types are accessible[1,2], which are a kind of organometallic compounds with greatly growing interest due to their potential application to asymmetric reaction catalysts[3,4]. As an efficient separation technique for enantioseparation which requires mild separation conditions, high performance liquid chromatography (HPLC) is considered to be the most efficient way to resolve the clusters with new-type chiral stationary phases (CSPs) without destruction of the clusters. In the present work, a new CSP was prepared by coating amylose tris(3,5-dimethylphenylcarbamate) (ADMPC) on small particle silica gel, and for the first time applied to the enantioseparation of some new chiral tetrahedral clusters with good results. The effects of various parameters on the retention factors and separation results were also investigated.
摘要:Aristolochic acid (AA) composed of AA-Ⅰ and AA-Ⅱ (Fig.1) is the major toxic component extracted from Aristolochia plants[1]. Recently, it has been proved by several researches that high doses of aristolochic acids (AA) can result in a severe kidney disease named Chinese herbs nephropathy (CHN)[2]. It is characterized by a progressive interstitial fibrosis leading to a severe atrophy of the proximal tubules[3]. In the past several years, CHN has been reported in many countries including Belgium, France, Spain, UK and Japan[1]. Owing to its high toxicity, several health institutions, including the US Food and Drug Administration (FDA), and Medicines Control Agency (MCA), have warned people to pay attention to the safety information about botanical products containing AA. Many countries including UK, Canada, Australia, and Germany have announced banning to restrict the importation, sale and use of AA-containing medicines. So it is of great significance to develop effective and rapid methods to quantify the content of AA in regular herbal medicines.
摘要:1 Micro chemical system on chip Micro integrated chemical systems are expected as promising ultra high throughput chemical and bio processors with extremely small volume. Our research groups have proposed and developed the original methodologies for micro integration of general chemical systems as well the electrophoresis analysis in which many groups of this micro technology are interested. They are as follows: (1) micro unit operation (MUO); (2) continuous flow chemical processing (CFCP); (3) 2D and 3D multi-phase laminar flow network; (4) thermal lens microscope (TLM).
摘要:Since their introduction in 1992 by Fréchet and Svec[1], monolithic supports as stationary phases in high performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) have gained significant interest due to a number of unique properties. Their ease of preparation, high reproducibility, versatile surface chemistry and fast mass transport are advantageous in a variety of applications[2-4]. Separations in diverse chromatographic modes have been performed in either HPLC or CEC, showing their strong point for high-speed separations of biological and synthetic molecules[5-12]. Although a number of papers have been reported on the application of monolithic supports as chiral stationary phases in CEC and pressure-assisted capillary electrochromatography (p-CEC)[13-19], few reports have so far been published on chiral monolithic stationary phases for liquid chromatography[20].
摘要:Bile acids are synthesized in the liver from cholesterol by the action of hepatic enzymes and excreted into the small intestine via the bile duct. In the intestinal lumen, they assist lipolysis and the absorption of fats by forming mixed micelles, and then return to the liver upon absorption in the ileum and proximal colon. Because of their efficient hepatic uptake, bile acids have low concentrations in the peripheral blood. Recent observations also indicate that the nuclear bile acid receptor regulates the bile acid pool by repressing transcription of genes encoding hepatocyte transporters[1] as well as cholesterol 7α-hydroxylase[2,3], which is the rate-limiting enzyme for bile acid biosynthesis.
摘要:Drugs in the body are bound to metabolizing enzymes, targets/receptors and transport proteins in certain extent. The binding of drugs to targets or receptors is mainly specific and responsible for its pharmacological and therapeutic effects. The metabolizing of drugs by enzyme involves both specific and non-specific binding. Drugs interact to a different degree with proteins in blood non-specifically, which affects the distribution, metabolism, elimination, and pharmacological action. These binding properties are characteristic for a particular drug. Therefore, characterization of protein binding of drugs is important not only in therapeutic drug monitoring but also in early drug development. The binding of drugs to various proteins has been extensively studied. However, drugs may interact with each other in these binding reactions. Simultaneous administration of drugs influences their protein binding behavior, subsequently their absorption, excretion, distribution, efficacy and toxicity, which has been observed in many cases such as warfarin and phenylbutazone[1], cefazolin and cefoperazone[2]. Depending on the concentrations and their relative affinities for the binding sites, one drug may compete with another and displace it from the binding sites. The purpose of this study is emphasized on the evaluation of drug interaction in binding to protein.
摘要:Since the development of solid phase micro-extraction (SPME) method[1], many modifications have been made to improve the availability and application of the technique[2-5]. The in-tube SPME (ITSPME) was emerged and employed in high performance liquid chromatography (HPLC) as an efficient and simple preparation method, which offers several advantages over the fiber SPME syringe[6]. The ITSPME should preserve the advantages of SPME, and could offer higher enrichment factor, better quantitation, and automation through an on-line coupling with a chromatograph.
摘要:Adenosine and its corresponding nucleotides adenosine 5′-monophosphate (AMP), adenosine 5′-diphosphate (ADP) and adenosine 5′-triphosphate (ATP) are important biomolecules that provide energy and substrates for various cellular biochemical processes[1]. There have been strong demands for sensitive and reliable analysis of these nucleotides because the determination of their levels in cells may provide valuable information for understanding cellular energy metabolism. Analysis of adenosine nucleotides is a big challenge because these chemicals exist together with high cellular background in samples. Moreover, nucleotides are extremely polar due to the presence of multiple phosphate groups that may interfere with chemical determination. In particular, the nucleotide phosphates are not retained under conventional reversed-phase chromatographic conditions because of their extremely high polarity[2]. The most common approach for quantitative analysis of nucleotide phosphates in cellular extracts is to determine indirectly the corresponding parent nucleosides resulted from enzymatic dephosphorylation after the nucleotides were separated by using an anion-exchange solid phase extraction. The generated nucleosides were analyzed by using liquid chromatography with ultra violet absorption detection (LC/UV), radio-immunoassay and liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS)[3-6]. Because nucleotides are not retained under conventional reversed-phase conditions, ion-suppression high performance liquid chromatography (HPLC)[7], capillary electrophoresis[8] and ion-pairing HPLC[9-11] have been employed to circumvent the poor retention problem. The high selectivity of MS and MS/MS techniques provides great separation and detection power, making them attractive alternatives for the trace analysis of nucleotides. The application of negative ion electrospray ionization (ESI)-MS to nucleotide analysis has been reviewed[12,13]. The use of negative ion ESI-MS seemed to be a logical starting point for nuc
摘要:Some traditional Chinese medicines (TCM) have a long history of common therapeutic use. Recently, an increased interest can be observed in the characterization of these natural substances in order to have a better control on their action in health protection. However, due to the complexity of their chemical composition, it is in most cases very difficult or even impossible to identify all the potentially active substances. Hence, usually only a very reduced number of the active components are determined, which does not always allow to evaluate the inherent quality of the products. Therefore, this lack of characterization possibilities is a strongly limiting factor towards their more general application.
摘要:Inverse chromatography (IC) has been widely applied to characterize surface, interface, and bulk characteristics of technologically important materials. Probe molecules with known properties are injected into an isothermal chromatographic system with the material of interest as stationary phase. The molecular interactions between chemicals and this material can be characterized from the retention of the probe chemicals. Linear solvation energy relationships (LSERs) have been successfully used for the characterization of molecular interactions involved in many partition[1] and adsorption[2,3] equilibria. In this study we combined the inverse liquid chromatography (ILC) and LSER method to characterize the molecular interactions between hydrophobic organic compounds (HOCs) and soils based on the retention factors of 28 probe HOCs, which were measured by soil column liquid chromatography (SCLC)[4-6].