Thin layer chromatography detection methods

Two-dimensional thin-layer chromatography. This method is used to verify the presence of terminal 5-sultones, terminal unsaturated y-sultone, and terminal 2-chloro-y-sultone, if they are detected in the gas chromatographic determination. After extraction of the neutral oil from the AOS sample, the neutral oil is made up volumetrically to at least a 10% solution in hexane. Of this solution 3 pi is spotted onto a silica gel TLC plate together with standard sultones. It is twice developed with 2-propyl ether and then after turning the plate 90° twice developed with 60/40 n-butyl chloride/methylene chloride. The... 

Some studies have evaluated the quantity of a specific constituent in various herbal products by a thin-layer chromatography spectrophotometric method. Of 44 feverfew products that were evaluated, 14 (32%) did not contain the minimum of 0.2% parthenolide content (active ingredient) and 10 (22%) did not contain any detectable levels of parthenolide [30]. 

Amino-terminated telechelic polybutadiene was prepared by LiAlH4 reduction of amidino end-group in polybutadiene, which was polymerised by a water-soluble initiator, 2,2 -azobis(amidinopropane)dihydrochloride. The structure was analysed by 1H- and 13C-NMR, but functionality of 2.0 was obtained by a titration method [70]. Synthesis of co-epoxy-functionalised polyisoprene was carried out by the reaction of 2-bromoethyloxirane with living polymer that was initiated with sec-butyl lithium. The functionality of the resulting polyisoprene was 1.04 by 1H-NMR and 1.00 by thin layer chromatography detected with flame ionisation detection [71]. 

Subsequently, thin layer chromatography (TLC) methods have been extensively evaluated to optimize the detection of laxatives/ The most important findings for the successful detection of laxatives by TLC were (1) the skill and experience of the operator, (2) the choice of the mobile phase (ethyl acetate toluene glacial acetic acid [4 16 1] and hexane toluene glacial acetic acid [3 1 1] gave the best results), and (3) use of high-performance TLC plates with a concentrating zone. 

Just like the physical and microchemical methods of detection, the indirect, biological-physiological detection procedures are very selective when apphed to thin-layer chromatography. Here it is not chemical functional groups or particular physical properties that are selectively detected but effects on highly sensitive biodetectors . The following detection techniques have been employed ... 

This volume is the second of a series of practice-orientated TLC/HPTLC books published in excellent quality by VCH Publishers. As in the first volume, a series of reagents and detection methods have been reviewed with the intention of helping the practical analyst increase the detection specificity of routine samples separated by thin-layer chromatography. 

The on-line principle has also been extended into the field of detection (Fig. 8). Thus, it is now possible to record FTIR [27-31] and Raman spectra in situ [32, 33], and there have been considerable advances in the on-line coupling of thin-layer chromatography with mass spectrometry. Here it has been, above all, the research groups of Wilson [34-36] and Busch [37-40] that have made the necessary instrumental and methodological advances, so that TLC must no longer be viewed as merely a clean-up method. Rather it forms the essential central point for all these on-line coupling techniques. 

Fig. 8 PossibUities for on-line coupling of thin-layer chromatography with physical measurement and determination methods. CCD = Charge Coupled Device Detection.

Jork, H., Funk, W., Fischer, W., Wimmer, H. Thin-layer Chromatography, Reagents and Detection Methods, Vol. 1 a, VCH-Verlagsgesellschaft, Weinheim, Cambridge, New York, 1990. 

Thin-layer chromatography has the great advantage that the result of the separation is stored — usually invisibly — on the TLC/HPTLC plate as on a diskette. In such cases it needs developing or detecting, rather like an exposed film. This can now be done online or off-line so that the analyst can decide which method to use to detect the separated substances. 

Reactions can be exploited more speciHcally if it is known that particular functional groups are present [cf. Chapter 2]. They still do not allow direct identification, but they increase the specificity of the evidence. The chromatographic separation carried out before detection also contributes to this. This reduces the number of potential components. However, this does not exclude the possibility that there might be several substances in the particular part of the chromatogram involved. This not only applies to thin-layer chromatography but also applies with equal force to other microanalytical separation methods (GC, HPLC). 

Thin layer chromatography reagents and detection methods / Hellmut Jork... -Weinheim New York Basel Cambridge Tokyo VCH. 

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