Thin-layer chromatography qualitative analysis

The multiplicity of responses makes thin-layer chromatography not particularly suited for pyrethrum analysis, either qualitative or quantitative. It did confirm, however, that the crude oleoresin contains several pyrethroid compounds in substantial quantity, as previously shown by gas chromatography work. 

The first part of the book consists of a detailed treatment of the fundamentals of thin-layer chromatography, and of measurement techniques and apparatus for the qualitative and quantitative evaluation of thin-layer chromatograms. In situ prechromatographic derivatization techniques used to improve the selectivity of the separation, to increase the sensitivity of detection, and to enhance the precision of the subsequent quantitative analysis are summarized in numerous tables. 

All previous discussion has focused on sample preparation, i.e., removal of the targeted analyte(s) from the sample matrix, isolation of the analyte(s) from other co-extracted, undesirable sample components, and transfer of the analytes into a solvent suitable for final analysis. Over the years, numerous types of analytical instruments have been employed for this final analysis step as noted in the preceding text and Tables 3 and 4. Overall, GC and LC are the most often used analytical techniques, and modern GC and LC instrumentation coupled with mass spectrometry (MS) and tandem mass spectrometry (MS/MS) detection systems are currently the analytical techniques of choice. Methods relying on spectrophotometric detection and thin-layer chromatography (TLC) are now rarely employed, except perhaps for qualitative purposes. 

The latest innovation is the introduction of ultra-thin silica layers. These layers are only 10 xm thick (compared to 200-250 pm in conventional plates) and are not based on granular adsorbents but consist of monolithic silica. Ultra-thin layer chromatography (UTLC) plates offer a unique combination of short migration distances, fast development times and extremely low solvent consumption. The absence of silica particles allows UTLC silica gel layers to be manufactured without any sort of binders, that are normally needed to stabilise silica particles at the glass support surface. UTLC plates will significantly reduce analysis time, solvent consumption and increase sensitivity in both qualitative and quantitative applications (Table 4.35). Miniaturised planar chromatography will rival other microanalytical techniques. 

Thin-layer chromatography (TLC)2 has become a valuable tool for the qualitative and semi-quantitative analysis of various organic and mor-... 

Injection volumes of 5pl were used for both sample solutions and comparison standards. Qualitative residue confirmation was accomplished with thin layer chromatography using silica gel. Plates were developed with 1% chloroform in n-heptane, and visualized with alkaline silver nitrate spray as the chromogenic agent. Alternatively, p,p5-DDT and p,p5-TDE were confirmed by treatment with 5% methanoic potassium hydroxide [40]. Partial confirmation of Dieldrin was achieved by fractionating the analysis solution on a Mills column, thus isolating Dieldrin in the second fraction [35],... 

Analysis of On-Site Wastewaters for Pesticides by Thin-Layer Chromatography. A field method to identify qualitatively and semi-quantitatively the pesticide constituents of a pesticide-laden wastewater was developed. The field method was developed using thin-layer chromatography (TLC). TLC gives a presumptive test for the presence of specific pesticides and within 30 minutes an estimate of their concentrations. TLC may also reveal the presence of unknown substances. The field application of thin-layer chromatography requires a skilled chemist, but no expensive equipment. The following protocol describes the on-site use of TLC. 

Thin-Layer Chromatography. Thin-layer chromatography was used for many of the compounds which are of interest for either qualitative or quantative analysis. These techniques were used primarily as screening methods to supplement other analytical methods. For some brominated compounds such as TRIS, the detection system reported by Hahn (9) was applicable. This method is based upon the reaction of fluorescein with elemental bromine released through peroxide oxidation. An evaluation in our laboratory of this detection system indicated that semi-quantitative results... 

Frangopol and Morariu have edited a seminar on procaine and related drugs, methods of analysis, and effects on cell membranes [29]. Items covered include studies on Romanian drugs by mass spectrometry and gas chromatography-mass spectrometry, quantitative and qualitative determination of procaine in biological samples, separation and quantitative thin layer chromatography determination of procaine... 

In earlier times, thin-layer chromatography (TLC), polyamide chromatography, and paper electrophoresis were the major separation techniques for phenolics. Of these methods, TLC is still the workhorse of flavonoid analysis. It is used as a rapid, simple, and versatile method for following polyphenolics in plant extracts and in fractionation work. However, the majority of published work now refers to qualitative and quantitative applications of high-performance liquid chromatography (HPLC) for analysis. Llavonoids can be separated. 

It has been demonstrated that ILMs are suitable for qualitative and quantitative analyses of low-molecular weight compounds of biological interest, for example, carbohydrates, vitamins and amino acids [38], and glycolipids [40]. ILMs were further used for fhe direct analysis of alkaloids, anesthetics and antibiotics, separated by thin-layer chromatography (TLC) [46]. For this purpose, the ILM was spotted onto the fractions on the TLC-plates and the complete plate was measured in MALDI MS without the need for additional pretreatment of the TLC-samples. The mass deviation inherently caused by the inhomogeneous surface of fhe TLC-plafe was balanced by using the... 

Qualitatively interpreted assays such as mucopolysaccharide electrophoresis (MPS-EP), urinary organic analysis and amino acid thin-layer chromatography (AA-TLC) are extremely important in biochemical genetics and yet are difficult to quality control. Some useful control measures often used include ... 

Gas-Liquid Chromatography. Gas-liquid chromatography (GLC) affords both a qualitative and, if adequate internal standards are used, a quantitative analysis of the products of lipolysis. It is necessary, however, first to isolate the acids by a suitable method and then to inject them as free acids or as esters. The partial glycerides can be isolated by thin-layer chromatography and can also be determined by GLC of suitable derivatives. The acid(s) remaining in the partial glycerides can be identified readily by GLC following transesterification. Jensen and co-workers have utilized these techniques in their studies of lipase specificity (Jensen et al 1964). 

Analysis. Dilute aqueous solutions of hydroxyhydroquinone turn blue-green temporarily when mixed with ferric chloride. The solutions darken upon addition of small amounts, and turn red with additions of larger amounts of sodium carbonate. Derivatives used for identification are the picrate, which forms orange-red needles (mp of 96°C), and the triacetate (mp 96—97°C). Thin-layer chromatography and liquid chromatography are well suited for the qualitative and quantitative estimation of hydroxyhydroquinone (93,94). 

Benzimidazole carbamates have generally been determined by HPLC (20,124-126), although other methods have been reported based on enzyme immunoassay (147) or in gas chromatography (124). The commercial availability of high-performance thin-layer chromatography (HPTLC) plates with layers of very different polarities has improved the sensitivity, selectivity, and analytical precision of TLC, which has led to a reconsideration of the use of this technique for qualitative and quantitative analysis (54). 

Thin layer chromatography has been used in qualitative and quantitative analysis of saccharin, when present in artificial sweetening agents, beverages, food and pharmaceuticals. Several systems have been used and are listed in table 5-... 

Lee et al. (1975) also qualitatively studied urinary metabolites of32P-labeled white phosphorus in rats. They used thin-layer chromatography (TLC) at 4 and 24 hours after a single oral dose to show that radioactive urinary metabolites consisted of two classes of compounds. One of the compounds corresponded to inorganic phosphate, the other compound was less polar and suggested an organic phosphate, although the composition of this class of metabolites was not determined. TLC analysis of liver extract also showed two classes of compounds with similar properties. 

G. Richard, P. Gataud, J. C. Arnaud, and P. Bore, Qualitative analysis of preservatives using high-performance thin-layer chromatography. In Cosmetic Analysis (P. Bore, ed.), Marcel Dekker, Inc., New York, 1985, p. 157. 

The amino acids in a protein hydrolysate can be conveniently separated for qualitative analysis by paper or thin-layer chromatography or by elec-... 

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