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V Danube Symposium on Chromatography Yalta, November 11-16, 1985

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V Danube Symposium on Chromatography Yalta, November 11-16, 1985 <> tf2*>2 4 23, V DANUBE SYMPOSIUM ON CHROMATOGRAPHY YALTA, NOVEMBER 11-16, 1985 ABSTRACTS NAUKA" ACADEMY OF SCIENCES OF THE USSR GENERAL AND TECHNICAL CHEMISTRY DiVISION THE SCIENTIFIC COUNCIL ON CHROMATOGRAPHY INSTITUTE OF PHYSICAL CHEMISTRY V DANUBE SYMPOSIUM ON CHROMATOGRAPHY YALTA, NOVEMBER 11-16, .1985 ABSTRACTS к "NAUKA" troc 5t3.5H V Danube Symposium on Chromatography. ABSTRACTS. И.: "Nauka", 1985. The volume contains short abstracts of plenary lectures,section papers and poster contributions presented at the V Danube Symposium on Chromatography, Proceedings of the Symposium reflect recent advances and prospects of further development in all branches of modern chromatographic techniques, including column liquid chromatography, gas chromatography, ion exchan­ ge, thin-layer chromatography, flow electrophoresis as well as equipment development. PROGRAM COMMITTEE K.I.Sakodynskii (chairman), B.G.Belenkii, V.G.Berezkin, G.A.Chikin, V.P.Chizhkov, V.A.Davankov, O.G.Larionov, K.H.Saldadze, G.V.Samsonov, A.A.Zhukhovitskii, P.P.Zolotarev (g) Institute of Physical Chemistry of the USSR Academy of Sciences, 1985 GENERAL PROBLEMS OF CHROMATOGRAPHY 001 QUANTIFICATION OF THE INFORMATION OF CHROMATOGRAPHIC RETENTION DATA FOR THE IDENTIFICATION OF ANALVTES КОЛИЧЕСТВЕННАЯ ОБРАБОТКА ПАРАМЕТРОВ ХРОКАТОГРАФИЧЕСКОГО УДЕРЖИВАНИЯ С ЦЕЛЬЮ ИДЕНТИФИКАЦИИ АНАЛИЗИРУЕМЫХ ВЕЩЕСТВ J.F.K.Huber, G.Reich., E.Kenndler, Vienna, Austria In qualitative analysis the nature of the components of a sample have to be determined. In principle two approaches can be usedt Identification by means of characteristic data and elucidation of the chemical structure. In the first approach the identity of species is determined by charac­ terizing the species by means of data. Comparison of the data allows to decide if two species are identical or not. Due to the limited precision and accuracy of the data such a decision can be made only with a certain probability. The capacity of an identification method depends on its discrimination power and can be described quantitatively by applying information theory. In chromatography the components are discriminated by the separation process and the retention data can be used for the characterization of the species. The identifica­ tion capacity of this method depends on the efficiency and selectivity of the separation process as well as on the probability distribution of the species occurring wi­ thin a given retention range. Quantification of the information content of the different modes of chroraato- graphy leads to the conclusion that single stage opera­ tion gives less than 9 bit and this means not a very high identification capacity. The identification capacity can be increased significan­ tly if multidimensional chromatography is applied. In this technique the sample is separated on a cascade of columns by transfering the effluent of a given column in frac­ tions to the columns of the next separation stage of the system. It is crucial that columns of different retention characteristics are used. Such columns, which are little correlated in retention, can be selected by pattern recog­ nition. If carried out in a proper way a high identifica­ tion capacity can be achieved by multidimensional chroma­ tography. 002. PL COMPUTER CHROMATOGRAPHY POSSIBILITIES AND APPLICATIONS: TWO EXAMPLES TO CAPILLARY GC AND HIGH PERFORMANCE TLC ВОЗМОЖНОСТИ ШИРОКОГО ПРИМЕНЕНИЯ КОМПЬЮТЕРОВ В ХРОМАТОГРАФИИ: ДВА ПРИМЕРА В КАПИЛЛЯРНОЙ ГХ И В ВЫСОКОЭФФЕКТИВНОЙ тех R.E.Kaiser, R.I.Rieder, Bad Duerkheira.FRG ON-line using a 10 megabyte small laboratory Personal Computer (Apple lie) one can improve gas and liquid chro­ matographic techniques remarkably. In the case of two series coupled capillary gas chroma­ tography system the laboratory computer changes the gas pressure between the two series coupled capillaries, digi­ tizes, stores, integrates and evaluates the chromatogram series of an unknown sample mixture. The computer commands 5 (or more) consecutive injections of the same sample and after the series of runs it can do either adjusting the chromatographic system to optimum polarity conditions for further routine analysis or offers multilevel qualitative and quantitative analysis of the GC sample. As a result at least four sets of retention index increments and in­ formation about peaks under peaks are given, thus offering a new chromatographic evaluation principle: Multi Chroma­ tography, MC. The pressure adjusting system between the capillaries is a digital controlled piezo electronic fluidix system and adjusts hydrogen pressure reproducible at the millibar level thus controlling flow at the microliter per minute level. This determines the residence time in polare and apolare capillaries and therefore changes retention index data for polare compounds for several hundred unites in the pressure ranges applicable. In the case of planar chromatography the computer con- trolls sampling, separation and quantitation on high per­ formance thin-layer plates. One of the surprising results is that HPTLC analysis now reaches the top of accuracy of all existing chromatographic techniques, although many chromatographers consider TLC as semiquantitative only. By total area quantitation in one mm wide tracks touching each other the lab computer offers a complete change of the quantitation techniques including automatic wide range calibration, which leeds to HPTLC in the sense of High Precision. The computer chromatography principles of the two examples mentioned and further possibilities are shown and will be discussed. 4 003 PL STATE AND TRENDS IN OPLC СОСТОЯНИЕ И ТЕНДЕНЦИИ В ТОНКОСЛОЙНОЙ ХРОМАТОГРАФИИ ПРИ ПОВЫШЕННОМ ДАВЛЕНИИ E.Tyihak, Budapest, Hungary The special possibilities of totally closed planar liquid chromatographic system were first realized by deve­ lopment of over-pressured-layer chromatography (OPLC) using a pressurized ultra-micro chamber. OPLC is a logical extension of the theory-and practice developed in HPLC to the field of planar liquid chromato­ graphy. However there are important differences between OPLC and HPLC. It is obvious that the development trends in OPLC are based upon these facts. The outstanding properties of chemically bonded phases on various chromatoplates were used in OPLC for the effi­ cient separation of different substance groups. Because of the complexity of the retention mechanism, it is possible to separate simultaneously compounds of a wide polarity range with excellent resolution and short reten­ tion times. Using a two-dimensional separation in OPLC the effi­ ciency increases quadratically. The versions of OPLC employ constant flow rate which has special advantages in the case of chromatoplates with concentrating zone. The extremely narrow line of substan­ ce that is formed at the interface provides an optimal start for chromatographic separation'. This separation mo­ de is especially attractive when larger sample amounts are applied. It is important that in this system very dilute solutions can be used, too. The overpressured multi-layer chromatography is a very attractive version of OPLC because a large number of samples can be separated at the same time. One- and two-dimensional on-line separation and detec­ tion in OPLC increase the efficiency of this technique and the application possibilities, alike. Preparative OPLC separation modes are more suitable for isolation of substances of different structure than the classical TLC. OPLC opens a new way in this field as the separation is many times faster in a pressurized chamber than in normal TLC chambers and so the diffusion of substances in the sorbent layer decreases dramatically. 004. MICROCOLUMN CHROMATOGRAPHY OF SYNTHETIC POLYMERS, PROTEINS AND THEIR FRAGMENTS МИКРОКОЛОНОЧНАЯ ХРОМАТОГРАФИЯ СИНТЕТИЧЕСКИХ ПОЛИМЕРОВ, БЕЛКОВ И ИХ ФРАГМЕНТОВ B.G.Belenkii, E.S.Gankina, V.G.Maltsev, Leningrad,USSR The application of exclusion and hydrophobic micro­ column chromatography to the analysis of synthetic poly­ mers, proteins, peptides and amino acids has been consl- 5 dered. Since a small amount of the eluent is used in columns 0,5 mm in diam. ( V » 50/ul) for exclusion chroma­ tography, it is possible to employ 'any solvents as eluents including expensive and toxic solvents. Spectrofotometric, fluorometric and refractometric detectors with the cell volume of O.l-l.O ml were used for the detection of the eluate in microcolumn chromatography. Steel and fluoroplastic microcolumns 0.5-1.0 mm in diam. with the efficiency of 40-70,10,J theoretical plates/m were used. Examples are presented of microcolumn exclusion chroma­ tography used for analysis of molecular-weight distribu­ tion of synthetic oligomers and polymers Including poly­ esters and polyamides and for the molecular-weight deter­ mination of peptides and proteins in the random coil con­ formation. The method of gradient microchromatographic analysis of DMS-amino acids with the aid of.a laser fluorimetric detector with a sensitivity of 10 mol was developed. 005. MICROCOLUMN SEPARATION METHODS I PAST, PRESENT AND FUTURE МЕТОДЫ МИКРОКОЛОНОЧНОГО РАЗДЕЛЕНИЯ: НАСТОЯЩЕЕ, ПРОШЛОЕ И БУДУЩЕЕ M.Novotny, Bloomington, Indiana, USA Whereas in the field of gas chromatography, the column miniaturization already started with the development of open tubular columns by M.J.E.Golay /1/, similar efforts in liquid chromatography (LC) can only be traced to the late 1970s. Encouraged by the theoretical considerations of Giddings /2/, as well as the successful efforts to decrease particle size in LC /3-5/, our laboratory pursued various
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