共查询到20条相似文献,搜索用时 15 毫秒
1.
Summary Propionamide-formaldehyde reaction products have been characterised using micellar electrokinetic chromatography (MEKC), HPLC-electrospray-MS
(HPLC-ES-MS) and time-of-flight-MS (TOF-MS). HPLC-MS-MS was used to distinguish between isomeric species. The MEKC separation
of all reaction products was obtained with good resolution and efficiency. Comparison of water-micelle distribution constants
(P
MEKC) for propionamide-formaldehyde with those for caprolactam-formaldehyde reaction products suggests that the concentration
of sodium dodecyl sulfate appropriate for use in MEKC is inversely related toP
MEKC. Quantification of all species containing one or two amide units was achieved using standard calibration, mass balance and
the assumption of identical absorption coefficients for the same functional groups in monomers and dimers. 相似文献
2.
Sajid Husain Ponnapalli Nageswara Sarma Sankarayya Swamy 《Journal of separation science》1995,18(7):422-424
A capillary GC method employing an internal standard has been developed and successfully used for quantitative determination both of the raw materials used for the manufacture of m-phenoxybenzaldehyde and for the components of the reaction mixtures obtained at various stages of the development of the process. A complete analysis can be performed in a single temperature programmed run. 相似文献
3.
Separation and partial characterization of Maillard reaction products by capillary zone electrophoresis 总被引:1,自引:0,他引:1
Capillary zone electrophoresis proved useful for separating small amounts of both charged and uncharged solutes that are otherwise difficult to analyse. A typical complex mixture that had previously resisted all analytical approaches, including reversed-phase separations, is the products arising from the reaction of free amino acids with aldehydic sugars (Maillard reaction products). By using capillary zone electrophoresis [untreated capillary 50 cm x 75 microns I.D., 18 kV, 0.02 mol/l phosphate buffer (pH 7.5)], a number of products resulting from the reaction of glucose or ribose with glycine, alanine and isoleucine were separated and partially characterized. They were separated (1) without derivatization (and profiles of compounds absorbing at 220 nm were obtained), (2) as phenylthiocarbamyl derivatives in a search for reactive amino groups and (3) after derivatzation with 2,4-dinitrophenylhydrazine in a search for a method for compounds with a free aldehydic group. Phenylthiocarbamyl derivatives were separated in 0.005 mol/l borate buffer (pH 9.6) at 20 kV and 25 microA. Separation of 2,4-dinitrophenylhydrazones was effected by electrokinetic micellar chromatography in the same apparatus using a 50 cm x 75 microns I.D. capillary at 10 kV in 0.01 mol/l Na2HPO4-0.006 mol/l tetraborate, 0.050 mol/l with respect to sodium dodecyl sulphate. The results are compared with those given by high-performance liquid and thin-layer chromatography. 相似文献
4.
Separation and analysis of DNA sequence reaction products by capillary gel electrophoresis 总被引:5,自引:0,他引:5
This paper demonstrates the potential of capillary gel electrophoresis with laser induced fluorescence detection as a tool for DNA sequence determination. Both synthetic oligonucleotides and single-stranded phage DNA were utilized as templates in the standard chain termination procedure. Primer molecules were tagged at the 5' end with the fluorescent dye, JOE. First, baseline resolution of a dA extended primer from 18 to 81 bases long, a total of 64 fragments, was observed. A second synthetic template was designed to yield alternating stretches of dA and dT extensions of the primer. Thirdly, the sequence reaction products from a synthetic oligonucleotide template containing all four bases was analyzed in four independent runs, one for each of the four base-specific reactions. In all cases, the expected number and patterns of peaks were observed by capillary gel electrophoretic analysis. Finally, separation of sequence reaction products generated with single-strand M13mp18 phage DNA as template exhibited baseline resolution of fragments differing in length by a single nucleotide and from 18 to greater than 330 bases total length. 相似文献
5.
6.
W. Zwickenpflug H. Wei? N. Fürst-Hunnius E. Richter 《Fresenius' Journal of Analytical Chemistry》1998,360(6):679-682
N-Nitroso-triazine herbicide species were synthesized as reference standards and their reaction products were separated by
TLC. The method was established for analytical as well as for preparative amounts to achieve a sufficient separation between
the educts, the byproducts and the N-nitrosated moieties. Separation of the reaction mixture was performed by two-dimensional
TLC, using different mobile phases for each dimension. In the second dimension two developments were executed using the same
solvent mixture. To examine the quality of performance, the separation zones were scrapped off, extracted and analyzed in
the HPLC-diode array detection (DAD) mode in comparison with standards of the educts and the products of their N-nitrosation.
This method minimizes the contact with the resulting N-nitroso compounds. At present nothing is known about the toxicological
relevance or risk assessment on human health of N-nitrosocyanazine or N-nitrosoterbuthylazine species. Therefore the practical
handling of these putative mutagenic and carcinogenic substances should be seen under the aspect of precaution and prevention
of contamination.
Received: 25 August 1997 / Revised: 13 October 1997 / Accepted: 21 October 1997 相似文献
7.
W. Zwickenpflug H. Weiß N. Fürst-Hunnius E. Richter 《Analytical and bioanalytical chemistry》1998,360(6):679-682
N-Nitroso-triazine herbicide species were synthesized as reference standards and their reaction products were separated by TLC. The method was established for analytical as well as for preparative amounts to achieve a sufficient separation between the educts, the byproducts and the N-nitrosated moieties. Separation of the reaction mixture was performed by two-dimensional TLC, using different mobile phases for each dimension. In the second dimension two developments were executed using the same solvent mixture. To examine the quality of performance, the separation zones were scrapped off, extracted and analyzed in the HPLC-diode array detection (DAD) mode in comparison with standards of the educts and the products of their N-nitrosation. This method minimizes the contact with the resulting N-nitroso compounds. At present nothing is known about the toxicological relevance or risk assessment on human health of N-nitrosocyanazine or N-nitrosoterbuthylazine species. Therefore the practical handling of these putative mutagenic and carcinogenic substances should be seen under the aspect of precaution and prevention of contamination. 相似文献
8.
A Series of barbiturates (I) has been permethylated with the methylsulfinylmethide carbanion and methyl iodide and the products (II to IV) separated, quantified and characterized by g.c.-m.s. The ratios and fragmentation patterns of II to IV are highly dependent upon the nature of the R-groups. All fragment ions have been confirmed by accurate mass measurements or perdeuteriomethylation. 相似文献
9.
Bailey PJ Coxall RA Dick CM Fabre S Parsons S Yellowlees LJ 《Chemical communications (Cambridge, England)》2005,(36):4563-4565
Treatment of dimethylmagnesium with bulky alpha-diimine ligands provides either the biradical methyl-bridged complexes [(alpha-diimine-.)Mg+(mu-CH3)]2 via single electron transfer (SET), or the product of methyl transfer to an imine carbon atom depending upon conditions. 相似文献
10.
Yang Weifan Yuan Shuangui Xiao Yonghou Xu Yanbing 《Journal of Radioanalytical and Nuclear Chemistry》2002,252(3):593-596
Protactinium was produced by the reaction of 60 MeV/nucleon 18O with natural uranium. A simple, relatively fast radiochemical procedure was developed, which can be used for the extraction separation of protactinium from uranium and from the complex reaction products using 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone and tri-iso-octylamine as extractants. Measurements of the gamma-ray spectra for the separated protactinium fractions were performed with a HPGe detector. The measured g-ray spectrum of protactinium shows that the decontamination from the main impurity elements, especially zirconium and niobium, is quite satisfactory. 相似文献
11.
It has been proved, by TLC and synthetic methods, that the odoriferous material formed in the reaction of cyclododecanone and phenyl ethylene glycol under acidic condition, was not the ketal of cyclododecanone, but an acetal of phenylacetaldehyde with phenyl ethylene glycol—the by-product formed from phenyl ethylene glycol. The cis-trans isomers of the acetal were separated by chromatography, the configurations were confirmed via the analysis of their 1H NMR spectra, and the odors were evaluated as well. 相似文献
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13.
Camera E Picardo M Presutti C Catarcini P Fanali S 《Journal of separation science》2004,27(12):971-976
We developed a simple and reliable analytical method for the quantification and the characterization of ceramides extracted from biological samples by high-performance liquid chromatography (HPLC) coupled to electrospray ionisation tandem mass spectrometry (ESI/MS/MS). The chromatographic separation of analytes was carried out in a RP8 column, eluting with a methanol-water mixture in gradient elution mode. The separated lipids were detected by total ion monitoring and characterised by MS/MS spectra; quantitative analysis was performed by integrating the extracted ion peaks obtained in the negative ion mode. Good repeatability was obtained for retention time (0.3-2%), peak area ratio (A(S)/A(IS), 2-8%), as well as limit of detection (LOD, 5-26 pg) and quantification (LOQ, 13-53 pg). The method was validated for the analysis of N-palmitoyl-D-erythro-sphingosine (Cer16), N-stearoyl-D-erythro-sphingosine (Cer18), N-tetracosanoyl-D-erythro-sphingosine (N24:0, lignoceric ceramide, Cer24:0), and N-tetracos-15'-enoyl-D-erythro-sphingosine (N24:1, nervonic ceramide, Cer24:1), giving good results. Lipid mixtures, extracted from skin and epidermal cells, were analysed for their content of the studied ceramides. 相似文献
14.
The identity of 45 protein spots representing 32 orthologues within the Ochrobactrum anthropi proteome within a gradient of pH 4-7, and mass range 5-90 kDa were determined across species boundaries. These proteins could be classified into 13 functional categories and establish metabolic, regulatory and translatory systems including amino acid biosynthesis, electron transport and the potential for plant symbiosis in a molecularly understudied organism. Amino acid composition and/or peptide mass fingerprinting were employed as a means to search the Swiss-Prot and OWL protein sequence databases for similarity within a broad taxonomic class of bacteria. Candidate matches from database searches could be compared and a simple multiplication matrix based on co-occurrence and rank within the top 96 most similar entries was used to provide statistical confidence. This mathematical matrix was evaluated with respect to the characterisation of O. anthropi, an unsequenced and understudied bacterium, in the light of the recent influx of DNA sequence information. 相似文献
15.
Guo-Feng Wang Hui-Juan Chu Hong-Liang Wei Xiao-Qian Liu Zi-Xuan Zhao Jing Zhu 《Chemical Papers》2014,68(10):1390-1399
The Diels-Alder reaction was used to fabricate hydroxypropyl methylcellulose-based hydrogels. First, hydroxypropylmethylcellulose (HPMC) was modified by a carboxyl-containing diene molecule (SFA) which was synthesised from furfurylamine and succinic anhydride. Second, dienophile groups were introduced into HPMC by the coupling reaction with N-maleoyl alanine (AMI) using N,N′-dicyclohexylcarbodiimide (DCC) and 4-dimethylaminopyridine (DMAP). Subsequently, the asprepared furan- and maleimide-modified HPMC were dissolved in water and gelation was observed at a pre-determined temperature after a period of time. The samples thus obtained were characterised by FTIR, NMR, SEM, etc. The gelation time changing with temperature, concentration of the solution, and solvent was measured. It was found that gelation time decreased with increasing temperature and concentration of the solution, and that water had a rate-accelerating effect on Diels-Alder reaction. The swelling behaviour indicates that the hydrogels have a high swelling ratio in water and the swelling ratio increases with the increasing temperature. Taking into consideration that the HPMC-based hydrogels are prepared under mild reaction conditions with an adjustable gelation time and thermal stability, the method described here has a potential application in biomaterials, especially in the areas of tissue-engineering and drug-controlled release carriers. 相似文献
16.
The products of the heterogeneous reactions of chlorine atoms and chlorine oxide radicals with acid coated Pyrex walls have been directly determined for the first time. Contrary to the usual assumption that chlorine atoms recombine to form Cl2, we find that the major product is HCl, with small amounts of perchlorate also formed. Similarly, ClO radicals form HCl rather than Cl2. The source of hydrogen for these reactions is probably the water always found in this type of vacuum system. These results may change the interpretation of flow tube experiments with chlorine atoms. Application to the H + HCl reaction is discussed as an example. 相似文献
17.
Grignard reactions with alkoxysilanes or carbonyl compounds produce alkoxymagnesium halides as by-products. Kinetic measurements for reactions of silanes and of a ketone were performed with Grignard reagents, enriched in alkoxymagnesium halides and taken in a great excess.The alkoxide-type reaction products complex tightly with Grignard reagents and enhance in this way their nucleophilicity, thus accelerating the reaction. However, alkoxides branched at α-C atom exert an unfavorable steric hindrance to reaction resulting in a decrease in the reaction rate. 相似文献
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Methylation is a crucial step in plant microRNA biogenesis. To improve our understanding of the methylation process and its regulation, a rapid and convenient high-throughput method should be sought to help with the study of reaction kinetics and assist the search for chemical inhibitors of the methyltransferase, HEN1. In this short communication, we report a pioneering work that used capillary electrophoresis (CE) to separate the miRNA and its methylation product. Capillary zone electrophoresis (CZE) with UV-absorption detection and a reduced running temperature achieved good separation of miR173/miR173* and miR173-m/miR173*-m with a detection limit of around 1 microM. To enhance detection sensitivity, capillary gel electrophoresis (CGE) coupled with laser-induced fluorescence (LIF) detection was also tested, and base-line separation of nanomolar duplex RNA samples was achieved using 4% polyvinylpyrrolidone (PVP) as the sieving matrix and SYBR Green II RNA gel stain for on-column labeling. Although further study is needed to investigate if the separation is sequence dependent, our study demonstrated, for the first time, that CE could be an effective and rapid method in monitoring the miRNA methylation process. 相似文献