Detection of multiple anions by thin-layer chromatography

A novel detection method for 21 different anions by thin-layer chromatography is presented. Anions on the target plate form salts with amine in a developing solvent and are visualized after staining with citric acid-acetic anhydride reagent as white spots contrasting against a pale red-pink background. This method has particularly high sensitivity for anions of chlorate, sulfate, phosphate, chromate and dichromate (0.02-0.05 microg). The method is demonstrated to efficiently detect toxic arsenite in curry sauce as an example application. The proposed method offers highly efficient indirect detection for a wide range of anions, and serves as a purification procedure for the preparation of anionic sample solutions for other analytical methods.     

Gas and liquid chromatography of hydrocarbons in edible vegetable oils.

Hydrocarbons, an important part of the minor constituents belonging to vegetable oils are reviewed. Their importance, origin, characterization and detection in edible vegetable oils are considered. The determination of some of them as a means of establishing oil quality and genuineness is also highlighted. The official methodologies, as well as the most commonly procedures used for isolation and analysis are reviewed. Furthermore, novel procedures applying new techniques for determining those compounds are also presented.     

Detection and determination of N-nitrosamines by thin-layer chromatography using fluorescamine.

A novel procedure is described for the detection and determination of N-nitrosamines (NAs) on thin-layer chromatographic plates. Ultraviolet irradiation of NAs on activated plates (silica gel or aluminum oxide) yields primary or secondary amines, which after spraying with fluorescamine reagent give fluorescent or non-fluorescent products, respectively. The majority of the 24 NAs examined afforded NAs, although the volatile dimethyl-, diethyl- and pyrrolidine-N-nitrosamines gave limits of 500, 40, and 40 ng, respectively. Spectrophotometric determinations of the relative fluorescence of 0.1-40 nmoles of NAs gave rise to nearly linear calibration curves when plotted on a log-log scale.     

Detection of sodium alkanesulphonates and alkylbenzenesulphonates by polyamide thin-layer chromatography.

A thin-layer chromatographic method was investigated in which two series of sodium alkanesulphonates (C4-C18) and alkylbenzenesulphonates (C0-C14) were separated. All of the compounds tested were clearly separated on polyamide layers with aqueous ammonia-pyridine and aqueous ammonia-pyridine-methanol systems and detected with high sensitivity by spraying with a pynacryptol yellow reagent and then observing under UV light (253.6nm).     

Detection of Actaea racemosa adulteration by thin-layer chromatography and combined thin-layer chromatography-bioluminescence

Actaea racemosa L. (black cohosh; syn. Cimicifuga racemosa L. Nutt.) is a native North American perennial whose root and rhizome preparations are commercially available as phytomedicines and dietary supplements, primarily for management of menopausal symptoms. Despite its wide use, methods that accurately identify processed A. racemosa are not well established; product adulteration remains a concern. Because of its similar appearance and growing locales, A. racemosa has been unintentionally mixed with other species of the genus, such as Actaea pachypoda Ell. (white cohosh) and more commonly Actaea podocarpa DC. (yellow cohosh). The genus Actaea also has 23 temperate species with numerous common names, which can also contribute to the misidentification of plant material. Consequently, a variety of Actaea spp. are common adulterants of commercially available black cohosh preparations. Thin-layer chromatography (TLC) and combined TLC-bioluminescence (Bioluminex) are efficient, economical, and effective techniques which provide characteristic patterns and toxicity profiles for each plant species. These data indicate that common black cohosh adulterants, such as yellow cohosh, can be differentiated from black cohosh by TLC and TLC-bioluminescence. This study also showed that unknown contaminants that were not detected using standard A. racemosa identity techniques were readily detected by TLC and TLC-bioluminescence.     

Antioxidant analysis in edible oils and fats by normal-phase high-performance liquid chromatography

Following a simple dilution in the appropriate phase, the sample is injected directly onto either of two normal-phase high-performance liquid chromatography systems (3,5-di-tert.-butyl-4-hydroxytoluene or 3-tert.-butyl-4-hydroxyanisole-tert.-butylhydroquinone) with UV detection at 280 nm. An isocratic ternary mobile phase, incorporating acetonitrile as the polar modifier, has been found to facilitate such an approach, thereby avoiding the discriminatory and recovery problems inherent in other techniques requiring prior sample manipulations. The three most commonly used antioxidants may be estimated at levels down to 3 ppm (3,5-di-tert.-butyl-4-hydroxytoluene or 3-tert.-butyl-4-hydroxyanisole) and 10 ppm (tert.-butylhydroquinone) within 30 min.     

The use of thin-layer chromatography in the analysis of lubricating oils

Summary A report is given on the application of thin-layer chromatography to the analysis of additives in lubricating oils. The separation and identification of antioxidants, phenates, sulphonates, zinc dialkyl dithiophosphates and polymeric additives is described. A measurement of additive depletion in used oils is possible by comparison of corresponding chromatograms.

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Zusammenfassung Es wird über die Verwendung der Dünnschicht-Chromatographie bei der Analyse der Additive von Schmierölen berichtet. Die Abtrennung und Identifizierung von Antioxydantien, Phenolaten, Sulfonaten, Zinkdialkyldithiophosphaten und polymeren Additiven wird beschrieben. Eine Messung der Abnahme der Additivkonzentration in gebrauchten Ölen ist durch Vergleich entsprechender Chromatogramme möglich.

     

Detection of organo-phosphorus pesticide residues in autopsy tissues by thin-layer chromatography

Summary Benzene is a suitable solvent for separation of ethyl parathion, methyl parathion, malathion, diazinon and meta-systox on silica gel thin layers. Rhodamine B is used as detection reagent. Other solvents are described which work almost as well, and which are superior for separation of mixtures of metabolites of some of these pesticides.

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Zusammenfassung Benzol eignet sich für die DC-Trennung von Äthylparathion, Methylparathion, Malathion, Diazinon und Metasystox auf Kieselgelplatten. Rhodamin B wurde als Nachweisreagens verwendet. Andere Lösungsmittel, die fast ebensogut geeignet sind und sich für die Trennung von Pestizidmetaboliten sogar besser eignen, wurden angegeben.

     

The determination of phenolic anti-oxidants in edible oils and fats by high-performance liquid chromatography

A simple procedure for the extraction of phenolic anti-oxidants with methanol is described. The extracted compounds are determined by gradient elution with retention times of 4.0–13.2 min; an internal standard technique is used for quantification.