Development of a new chromogenic spray reagent for the detection and identification of synthetic pesticide carbaryl in biological material by high-performance thin-layer chromatography

JPC – Journal of Planar Chromatography – Modern TLC -     

Qualitative and quantitative analysis of uric acid,creatine and creatinine together with carbohydrates in biological material by HPTLC

Summary In clinical diagnosis creatine, creatinine and uric acid are important parameters for the evaluation of renal diseases, and are partially responsible for gout and the formation of renal calculi. The determination of various carbohydrates, especially glucose, in urine and serum serves as an indicator of diabetes and other carbohydrate anomalies. A simple, rapid and economic method for the simultaneous screening and quantitation of these compounds is presented. No sample preparation is necessary for the determination in urine or in serum. The proposed method consists of separations on an amino modified HPTLC precoated plate. The detection of all relevant substances is reproducibly performed by simply heating the chromatogram to give stable fluorescent derivatives. The detection limits in all cases lie significantly below the physiological range.     

Development and validation of stability indicating RP-HPLC and HPTLC for determination of Niclosamide in bulk and in synthetic mixture

Two simple, specific, sensitive, accurate and precise stability indicating methods were described for quantitative determination of the anthelmintics drug Niclosamide. The first method was high performance liquid chromatographic with the use of a reversed phase hibar^R C-18 column (250 mm × 4.66 mm, 5 μm) and mobile phase of methanol: 1 mM ammonium phosphate buffer (85:15 v/v) at a flow rate of 1.2 mL/min. The retention time of drug was found to be 6.45 ± 0.02 min. Quantification of drug was achieved with diode array detection (DAD) at 332 nm. Linear calibration curve was obtained in concentration range 0.01–100 μg/mL with r² value of 0.999. The limit of detection and limit of quantification were found to be 0.048 μg/mL and 0.01 μg/ml respectively. The second method involved a high performance thin layer liquid chromatographic. Chromatographic separation was carried out with precoated silica gel G60 F254 aluminum sheets using toluene:ethyl acetate (7:3% v/v) as a mobile phase. Linearity of proposed method was found to be 200–700 ng/band at 332 nm with retention factor of 0.59 and r² value of 0.998. The limit of detection and limit of quantification were found to be 36.21 ng/band and 109.7 ng/band respectively. Both the developed methods were successfully validated as per International Conference on Harmonization guideline (ICH). Niclosamide was subjected to different stress conditions. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time. Stress samples were successfully assayed by developed high performance liquid chromatographic and high performance thin layer liquid chromatographic method. Statistically analysis proves that there were no statistical significant differences between two developed methods.     

Determination of glutathione in biological material by high-performance liquid chromatography with electrochemical detection

Glutathione in biological samples is extracted by perchloric acid and separated by ion-paier chromatography on a RP-18 phase. In a post-column reaction, glutathione is converted to an isoindole derivative by reaction with o-phthalaldehyde and detected at a galssy carbon electrode at 800 mV v. Ag/AgCl/3 M KCl. The detection limit is 40 pmol of glutathione injected.     

TLC technique for the detection and determination of gamma- BHC in biological material

Summary Five isomers present in technical benzene hexachloride were successfully separated by TLC on silica-gel G impregnated with silver nitrate solution. The -isomer was identified by running a control sample of -BHC. Measurement of the spot area was found suitable for the estimation of 5–20g of-BHC, and was applied to analysis of autopsy tissues. The limit of identification is 0.1g.

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Zusammenfassung Auf mit Silbernitratlösung imprägniertem Kieselgel G konnten dünn-schichtchromatographisch fünf Isomere aus technischem Hexachlorbenzol erfolgreich getrennt werden. Das-Isomere wurde mit Hilfe einer Vergleichsprobe identifiziert. Die Planimetrie der Flecken eignet sich zur Schätzung von 5–20 g-Hexachlorbenzol. Die Methode wurde zur Untersuchung von Autopsieproben angewendet. Die Nachweisgrenze beträgt 0,1g.

     

Microdetermination of lead in biological material

Summary Two photometric methods for the microdetermination of lead are described. The first is based on a one-color dithizone procedure and the accuracy is mostly sufficient for analyses of biological material such as urine. A more sensitive and accurate determination can be made with the reagent di--naphthylthiocarbazone.The samples are mineralized with the aid of nitric acid, hydrogen peroxide and potassium chlorate. Urine samples are concentrated through evaporation in vacuum before decomposition.

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Zusammenfassung Es werden zwei photometrische Methoden zur Mikrobestimmung von Blei beschrieben. Die erste beruht auf der Farbreaktion mit Dithizon unter Ausschaltung von dessen Eigenfarbe. Ihre Genauigkeit ist in der Regel für die Untersuchung von biologischem Material (wie etwa Harn) ausreichend. Ein empfindlicheres und genaueres Verfahren kann mit Hilfe von Di--naphthylthiocarbazon durchgeführt werden.Das Untersuchungsmaterial wird mittels Salpetersäure, Wasserstoffperoxyd und Kaliumchlorat mineralisiert. Harn wird vor der Mineralisierung im Vakuum eingedampft.

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Résumé On décrit deux méthodes colorimétriques pour le microdosage du plomb. La première repose sur la réaction colorée avec la dithizone par élimination de sa couleur propre. En général, la précision est suffisante pour la recherche dans les substances biologiques (comme l'urine). Un procédé plus sensible et plus précis peut s'effectuer à l'aide de la di--naphthylthiocarbazone. La prise d'essai est minéralisée au moyen de l'acide azotique, de l'eau oxygénée et du chlorate de potassium. L'urine est évaporisée dans le vide avant la minéralisation.

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With 2 figures.     

Evaluation of various biological activities of natural compounds by TLC/HPTLC

Abstract

Over the last years, thin layer chromatography (TLC) has become an increasingly important tool in the analysis of natural compounds, being used not only as a simple method of separation, identification, and quantitative determination of natural constituents, but also as a method for evaluating the potential applications of the separated compounds, different bioassays being compatible with TLC. This is due to the TLC advantages, of which could be mentioned: the possibility to simply, quickly, and flexibly analyze many samples in parallel, without the need for special steps of sample purification, obtaining visual results, and the possibility of multiple detections, all of these being achieved at very low costs. Considering these, the aim of this study is to give an overview on the application of TLC in evaluation of different biological activities of natural compounds, focusing on antioxidant, enzymatic, antimicrobial, and hormonal activities.     

Electrochemiluminescence detection of dichlorvos pesticide in luminol-CTAB medium

A simple, novel electrochemiluminescence (ECL) method for the detection of dichlorvos pesticide (DDVP) with high sensitivity was discovered. Detection was carried out in a static ECL system, in which a glassy carbon electrode was selected as the working electrode. ECL parameters, including the concentrations of cetyrltrimethylammonium bromide and luminol, the solution pH, and the scan rate of the applied potential, were optimized. Under these optimal conditions, the linear response of ECL-emission versus DDVP concentration was valid in the range 5-8000 ng/L (r(2)=0.9982) with a relative standard deviation of 4.3% at 2000 ng/L (n=10), yielding a detection limit (S/N=3) of 0.42 ng/L. The ECL emission was caused by a radical reaction process, in which the dissolved oxygen in the luminol solution reacted with the DDVP and generated free radicals. The free radicals reacted with the luminol anion and yielded the luminol radical. The approach presented was successfully applied to the determination of DDVP residues in vegetable samples.     

Developments in the production of biological and synthetic binders for immunoassay and sensor-based detection of small molecules

The need for chemical and biological entities of predetermined selectivity and affinity towards target analytes is greater than ever, in applications such as environmental monitoring, bioterrorism detection and analysis of natural toxin contaminants in the food chain.In this review, we focus on advances in the production of specific binders, in terms of both natural entities (e.g., antibodies) and synthetic binders (e.g., molecularly-imprinted polymers). We discuss the potential of emerging technologies for integration into immunoassay and sensing techniques. We place special emphasis on use of these technologies in bioanalytical applications.     

Development of multivalent macromolecular ligands for enhanced detection of biological targets

Macromolecular conjugates enable simultaneous binding of multiple ligands on one biological entity and these polyvalent interactions can be collectively stronger than the corresponding monovalent ligands. We have synthesized macromolecules and conjugated them with a lectin (Helix Pomatia lectin, HPA), and an antibody, both with shown affinities to certain bacteria. The binding ability was studied by flow cytometry and the results showed that the affinity of the biomolecules was greatly enhanced due to the polyvalent effect.     

Detection of intake of hashish in biological material

In order to detect hashish intake, urine, blood and serum were analysed for the main components of hashish, i.e., tetrahydrocannabinol (THC), cannabidiol, cannabinol and the decomposition product of THC, THC-carboxylic acid. After extraction and silylation, the samples were analysed by gas chromatography-mass spectrometry with multiple ion detection. The Emit-st-system is used as a pretest for urine.     

Limit of detection for the determination of Pt in biological material by RNAA using electrolytic separation of gold

Neutron activation analysis based on the¹⁹⁹Au indicator for platinum requires the separation of gold at high radiochemical purity. The limit of detection is strongly affected by the presence of gold; with a gold content of 50 pg/g, irradiating for 5 days at 5·10¹³ n/cm²s is needed to achieve a limit of detection of approximately 30 pg/g. In this case the nuclear interference from gold will exceed the level of platinum by several orders of magnitude and has to be determined with exceedingly high precision. Preliminary results for SRM 1577 Bovine Liver with 95% yield gave consistent results for Au, but Pt could not be detected.     

硼酸官能化金属-有机骨架磁性纳米复合材料的制备及其在茶叶农药残留检测中的应用

在茶叶的农药残留检测中,茶多酚及色素具有很强的基质效应,严重影响了色谱检测结果.该文将Fe3O4磁性纳米粒子与硼酸官能化金属有机骨架(BA-MOF)材料相结合,制备出一种对茶多酚等基质具有高效捕获能力的吸附材料Fe3O4@BA-MOF.结合气相色谱-质谱联用技术,建立了一种茶叶样品中农药残留的有效分析方法.通过在金属有...     

Development of a HPTLC method for in-process purity testing of pentoxifylline

A HPTLC method for the separation and identification of pentoxifylline and related substances, impurities of reaction partners, and side reaction products has been developed using different mobile and stationary phases. For quantitative assay of possible by-products as impurities, LiChrospher RP-18 F254s chromatoplates, acetone-chloroform-toluene-dioxane (2:2:1:1 v/v) as a mobile phase, and detection at 275 nm were employed. Linearity (r > or = 0.997), recovery (86.5-115.5%), and determination limit (0.1-0.6%) were evaluated and found to be satisfactory. This method enables monitoring of the synthesis, as well as purity control of pentoxifylline-containing raw materials and pharmaceuticals.