scholarly journals Analysis of Glimepiride in Human Blood and Urine by Thin Layer Chromatography and UV Spectrophotometry

2015 ◽  
Vol 20 (2) ◽  
pp. 71-75
Author(s):  
Mareta Mukharbekovna Ibragimova ◽  
Latif Tulaganovich Ikramov
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Whole Blood ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Chloroform Solution ◽  
Analytical Techniques ◽  
Uv Spectrophotometry ◽  
Limit Of Quantification ◽  
Layer Chromatography

Objective: An increasing numbers of cases of poisonings by glimepiride, either attempted suicide or accidental, combined with the absence of reliable methods for the detection and quantitation of glimepiride in biological matrices is the basis for the need for the development of new analytical techniques for forensic analysis.Materials and Methods: Analyses were performed using drug- free biological fluids (whole blood and urine). Specimens were spiked with chromatographically pure glimepiride. After hydrolysis with diluted hydrochloric acid at 50-60 °C for 15-20 min and a double extraction into chloroform, glimepiride was identified by thin-layer chromatography. Standard solution of glimepiride (1 mg/mL) and Sorbfil chromatographic plates were used for thin-layer chromatography. The thin-layer chromatography studies showed that the best mobile phase was chloroform:acetone (9:1), Rf value of glimepiride in five examinations was 0.37±0.02. Visualization of glimepiride was achieved byspraying with Dragendorff’s, Bushard’s, or diphenylcarbazone-chloroform solution followed by mercuric sulphate. The limit of detection of pure glimepiride by thin-layer chromatography was 0.5 p/mL, 1.5 p g/mL in whole blood and 1.0 p g/mL in urine. For spectrophotometric determinations of glimepiride, a UV/VIS spectrophotometer with 1 cm matches quartz cell was used. Standard solutions of glimepiride in ethanol were prepared at concentrations of 1-50 p g/mL and scanned in full-scan mode between 200-400 nm.Results and Conclusion: The wavelength maxima for glimepiride was found to be 227 nm with molar absorptivity of 3.2685x10 4 l/mol/cm. Beer’s law was obeyed in the concentration range of 2-40 p g/mL. The limit of detection and limit of quantification were found to be 0.97 p g/mL and 2.70 p g/mL, respectively. The results have been successfully applied in blood of patients after oral administration and on postmortem blood in an overdose death.Keywords: Glimepiride, Thin-layer chromatography, Spectrophotometry.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

scholarly journals Visualization of Aspalathin in Rooibos (Aspalathus linearis) Plant and Herbal Tea Extracts Using Thin-Layer Chromatography

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 938 ◽  
Author(s):  
Emily Amor Stander ◽  
Wesley Williams ◽  
Fanie Rautenbach ◽  
Marilize Le Roes-Hill ◽  
Yamkela Mgwatyu ◽  
...  
Keyword(s):  
Quality Control ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Throughput Screening ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Herbal Tea ◽  
Limit Of Quantification ◽  
Aspalathus Linearis ◽  
Layer Chromatography

Aspalathin, the main polyphenol of rooibos (Aspalathus linearis), is associated with diverse health promoting properties of the tea. During fermentation, aspalathin is oxidized and concentrations are significantly reduced. Standardized methods for quality control of rooibos products do not investigate aspalathin, since current techniques of aspalathin detection require expensive equipment and expertise. Here, we describe a simple and fast thin-layer chromatography (TLC) method that can reproducibly visualize aspalathin in rooibos herbal tea and plant extracts at a limit of detection (LOD) equal to 178.7 ng and a limit of quantification (LOQ) equal to 541.6 ng. Aspalathin is a rare compound, so far only found in A. linearis and its (rare) sister species A. pendula. Therefore, aspalathin could serve as a marker compound for authentication and quality control of rooibos products, and the described TLC method represents a cost-effective approach for high-throughput screening of plant and herbal tea extracts.

scholarly journals Techniques of quantitative evaluation of verapamil content in whole blood

2020 ◽  
Vol 19 (5-6) ◽  
pp. 116-121
Author(s):  
Alexander V. Voronin
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Whole Blood ◽  
Pharmacological Therapy ◽  
Gas Chromatography Mass Spectrometry ◽  
Calibration Model ◽  
Uv Spectrophotometry ◽  
Forensic Chemistry ◽  
Blood Samples ◽  
Layer Chromatography

Verapamil is a drug that can be toxic in pharmacological therapy and in case of misuse. Simple and informative methods of Verapamil quantification for forensic chemistry and hospital toxicology are needed. Aim. The objective of the study was to compare analytical potential of different methods for Verapamil quantification used in forensic chemistry and hospital toxicology. Materials and methods. The subject study was whole blood samples containing Verapamil. Verapamil in the blood samples was identified by gas chromatography-mass-spectrometry. Verapamil was quantified by thin-layer chromatography with videodensitometry and UV-spectrophotometry. Results. To quantify Verapamil content, the plates were scanned, the chromatogram images were processed and calibration models were given by means of computer program. The calibration model is described by polynomial (square) regression. In UV-spectrophotometry absorbance of samples at the wavelength of 277 nm was measured; blank blood extracts as a zero reference were used. The limits of quantifation for thin-layer chromatography with videodensitometry and UV-spectrophotometry were 300,0 and 6000,0 ng/ml respectively. The accuracy and precision for thin-layer chromatography with videodensitometry failed to exceed 20.2 и 24.3% respectively; for UV-spectrophotometry they were 27.5 и 7.4%. Conclusion. The ranges of quantifation make it possible to use thin-layer chromatography with videodensitometry for forensic chemistry and hospital toxicology. UV-spectrophotometry can be used to quantify Verapamil content in blood samples at the lethal concentration range.

scholarly journals Identification and quantification of glucose degradation products in heat-sterilized glucose solutions for parenteral use by thin-layer chromatography

PLoS ONE ◽  
2021 ◽  
Vol 16 (7) ◽  
pp. e0253811
Author(s):  
Sarah Leitzen ◽  
Matthias Vogel ◽  
Anette Engels ◽  
Thomas Zapf ◽  
Martin Brandl
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Parenteral Administration ◽  
Hptlc Plate ◽  
Limit Of Quantification ◽  
Glucose Degradation Products ◽  
Layer Chromatography ◽  
Hptlc Method

During heat sterilization of glucose solutions, a variety of glucose degradation products (GDPs) may be formed. GDPs can cause cytotoxic effects after parenteral administration of these solutions. The aim of the current study therefore was to develop a simple and quick high-performance thin-layer chromatography (HPTLC) method by which the major GDPs can be identified and (summarily) quantified in glucose solutions for parenteral administration. All GDPs were derivatized with o-phenylenediamine (OPD). The resulting GDP derivatives (quinoxalines) were applied to an HPTLC plate. After 20 minutes of chamber saturation with the solvent, the HPTLC plate was developed in a mixture of 1,4-dioxane-toluene-glacial acetic acid (49:49:2, v/v/v), treated with thymol-sulfuric acid spray reagent, and heated at 130°C for 10 minutes. Finally, the GDPs were quantified by using a TLC scanner. For validation, the identities of the quinoxaline derivatives were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Glyoxal (GO)/methylglyoxal (MGO) and 3-deoxyglucosone (3-DG)/3-deoxygalactosone (3-DGal) could be identified and quantified in pairs, glucosone (2-KDG), 5-hydroxymethylfurfural (5-HMF), and 3,4-dideoxyglucosone-3-ene (3,4-DGE) each individually. For 2-KDG, the linearity of the method was demonstrated in the range of 1–50 μg/mL, for 5-HMF and 3,4-DGE 1–75 μg/mL, for GO/MGO 2–150 μg/mL, and for 3-DG/3-DGal 10–150 μg/mL. All GDPs achieved a limit of detection (LOD) of 2 μg/mL or less and a limit of quantification (LOQ) of 10 μg/mL or less. R2 was 0.982 for 3.4-DGE, 0.997 for 5-HMF, and 0.999 for 2-KDG, 3-DG/3-DGal, and GO/MGO. The intraday precision was between 0.4 and 14.2% and the accuracy, reported as % recovery, between 86.4 and 112.7%. The proposed HPTLC method appears to be an inexpensive, fast, and sufficiently sensitive approach for routine quantitative analysis of GDPs in heat-sterilized glucose solutions.

scholarly journals ISOLATION AND DETERMINATION CARPAINE ALKALOID IN PAPAYA (CARICA PAPAYA L.) LEAF EXTRACT BY THIN-LAYER CHROMATOGRAPHY SCANNER

2021 ◽  
pp. 234-238
Author(s):  
YASMIWAR SUSILAWATI ◽  
NYI MEKAR SAPTARINI ◽  
ZELIKA MEGA RAMADHANIA ◽  
ELI HALIMAH ◽  
NAILAH NURJIHAN ULFAH
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Leaf Extract ◽  
Carica Papaya ◽  
Limit Of Detection ◽  
Preparative Thin Layer Chromatography ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Dragendorff Reagent ◽  
Layer Chromatography

Objective: This research was conducted to isolate the alkaloid carpaine by chromatography method and to determine it quantitatively by Thin Layer Chromatography Scanner. Methods: Dried leaves were macerated with ethanol 70% and fractionated with dichloromethane. Isolation of carpaine alkaloid from the dichloromethane fraction was carried out by column chromatography and preparative thin-layer chromatography according to the Rf value in Thin Layer Chromatography (TLC) after exposure by Dragendorff reagent. Results: The content of carpaine alkaloid was 7.5 mg with Rf 0.58 and dichloromethane: methanol (9.2:0.8) as eluent. Validation showed the linearity (R2) 0.9988, the limit of detection(LOD) was 0.05 ppm, the Limit of Quantification (LOQ) was 0.19 ppm, the recovery from 98.93-102.43%, and the % coefficient of variation was 0.16%. Conclusion: Carpaine alkaloid in papaya leaf extract was 10.52%.

Rapid Quantitation and Confirmation of Aflatoxins in Corn and Peanut Butter, Using a Disposable Silica Gel Column, Thin Layer Chromatography, and Gas Chromatography/Mass Spectrometry

1984 ◽  
Vol 67 (5) ◽  
pp. 973-975 ◽  
Author(s):  
Mary W Trucksess ◽  
William C Brumley ◽  
Stanley Nesheim
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Peanut Butter ◽  
Chloroform Solution ◽  
Fused Silica ◽  
Ion Source ◽  
Negative Ion ◽  
Gas Chromatography Mass Spectrometry ◽  
Layer Chromatography

Abstract Asimple, rapid, and solvent-efficient method for determining aflatoxins in corn and peanut butter is described. Aflatoxins B1, B2, G1, and G2 were extracted from SO g sample with 200 mL methanol-water (85 + 15). A portion of the extract was diluted with 10% NaCl solution to a final concentration of 50% methanol, and then defatted with hexane. The aflatoxins were partitioned into chloroform. The chloroform solution was evaporated, and the residue was placed on a 0.5 g disposable silica gel column. The column was washed with 3 mL each of hexane, ethyl ether, and methylene chloride. Aflatoxins were eluted with 6 mL chloroform-acetone (9 + 1). The solvent was removed by evaporation on a steam bath, and the aflatoxins were determined using thin layer chromatography (TLC) with silica gel plates and a chloroform-acetone (9 + 1) developing solvent. Overall average recovery of aflatoxin B] from corn was 82%, and the limit of determination was 2 ng/g. For mass spectrometric (MS) confirmation, aflatoxin B1, in the extract from 3 g sample (20 ng/g) was purified by TLC and applied by direct oncolumn injection at 40°C into a 6 m fused silica capillary gas chromatographic column. The column was connected directly to the ion source. After injection, the temperature was rapidly raised to 250¯C, and the purified extract was analyzed by negative ion chemical ionization MS.

Selection of a Simple and Sensitive Method for Detecting Zearalenone in Corn

1994 ◽  
Vol 77 (4) ◽  
pp. 939-941 ◽  
Author(s):  
Nora M Quiroga ◽  
Inés Sola ◽  
Edith Varsavsky
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Lead Acetate ◽  
Limit Of Detection ◽  
Acetate Solution ◽  
Average Recovery ◽  
Lead Acetate Solution ◽  
Layer Chromatography ◽  
Selection Of ◽  
Sensitive Method

Abstract A simple, rapid, and sensitive method for determining zearalenone in corn was selected. The toxin was extracted from 50 g test portions with 180 mL acetonitrile and 20 mL 4% KCl solution. A portion of the extract was defatted with isooctane. The acetonitrile extract was cleaned up with 20% lead acetate solution. The zearalenone was partitioned into toluene. The toluene solution was dried, and the residue was redissolved in benzene. The toxin was determined by thin-layer chromatography with silica gel plates and chloroform–acetone (9 +1) as the developing solvent. The overall average recovery of zearalenone from corn was 97%. The limit of detection was 50 μg/kg; this limit may be lowered by using fast violet B salt as spray reagent. The method was compared with 2 previous methods that determine zearalenone in biologically contaminated corn.

scholarly journals Quantitative Determination of Triterpenes from Amphiptherygium adstringens by Liquid Chromatography and Thin-Layer Chromatography and Morphological Analysis of Cuachalalate Preparations

2006 ◽  
Vol 89 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Andrés Navarrete ◽  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Xiuhong Ji ◽  
Paul Hersh ◽  
...  
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Gastric Ulcers ◽  
Array Detector ◽  
Plant Materials ◽  
Relative Standard ◽  
Layer Chromatography

Abstract Amphiptherygium adstringens (Anacardiaceae/Julianaceae), local name cuachalalate, is used in folk medicine for the treatment of cholelithiasis, fevers, fresh wounds, hypercholesterolemia, gastritis, gastric ulcers, and cancer of the gastrointestinal tract. The development of column high-performance liquid chromatographyphotodiode array detector (LC-PDA) and high-performance thin-layer chromatography (HPTLC)densitometry methods for the determination of masticadienonic acid and 3-hydroxymasticadienonic acid in cuachalalate preparations is described in this paper. Good separation of the compounds could be achieved by both methods. Either might be preparable depending on the requirements. The LC separation was performed on a Phenomenex Synergi MAX-RP 80A reversed-phase column operated at 40C with detection at 215 nm. The plant materials were extracted with methanol by sonication. The triterpenes present in the plant material and commercial extracts were separated with an acetonitrilewater reagent alcohol isocratic system. The limit of detection was 0.10.2 g/mL. The relative standard deviation values for the determination of triterpenes in plant extracts were less than 1.00%. This is the first report of an analytical method developed for the quantitative analysis of triterpenes from Amphiptherygium adstringens by LC-PDA and HPTLC. The stem bark showed higher amounts of triterpenes, and low amounts in root and stem root. The microscopic description of the crude drug of cuachalalate was also provided.

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