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

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.

Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb

<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>


Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 938 ◽  
Author(s):  
Emily Amor Stander ◽  
Wesley Williams ◽  
Fanie Rautenbach ◽  
Marilize Le Roes-Hill ◽  
Yamkela Mgwatyu ◽  
...  

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.


2015 ◽  
Vol 20 (2) ◽  
pp. 71-75
Author(s):  
Mareta Mukharbekovna Ibragimova ◽  
Latif Tulaganovich Ikramov

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.


2006 ◽  
Vol 89 (4) ◽  
pp. 995-998 ◽  
Author(s):  
Magdalena Wójciak-Kosior ◽  
Agnieszka Skalska ◽  
Grażyna Matysik ◽  
Magdalena Kryska

Abstract In this paper, a high-performance thin-layer chromatography (HPTLC) method combined with densitometry has been described. Chromatography was performed on silica gel Si 60F254 plates using dichloromethaneethyl acetateformic acid (9.5 + 0.5 + 0.1, v/v) mobile phase. This method has been successfully applied for the determination of phenobarbital in pharmaceuticals. Obtained results were comparable with traditionally used column high-performance liquid chromatography (HPLC) methods. For the proposed procedure, linearity (r &gt; 0.999), sensitivity (limit of detection 0.4 g/spot), recovery (97.8102.1%), and repeatability were found to be satisfactory. The HPTLC-densitometry method has many advantages, such as simplicity, reasonable sensitivity, rapidity, and low cost, and it can be successfully used in routine quality control of multidrug preparations containing barbiturates.


Proceedings ◽  
2018 ◽  
Vol 9 (1) ◽  
pp. 22
Author(s):  
Debanchal Dutta ◽  
Soumyajit Das ◽  
Manik Ghosh

A simple, rapid, precise and accurate High-Performance Thin Layer Chromatography (HPTLC) method was developed and validated for the estimation of Nintedanib, a novel tyrosine kinase inhibitor used in idiopathic pulmonary fibrosis, in bulk drug. Chromatography was carried out using silica gel 60 F254 Thin Layer Chromatography (TLC) plate and mobile phase Chloroform: Methanol in the ratio 7:3 v/v. The densitometric determination was done at 386 nm. Regression analysis data for the calibration plot were indicative of a good linear relationship between response and concentration over the range of 800–3200 ng/band. The variance (r) was found to be 0.999. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found to be 83.357 ng/band and 252.599 ng/band respectively. The method was validated according to the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use [ICH Q2(R1)] guideline. The method was precise and accurate with %RSD 0.5323 (intraday) and 0.6939 (interday) respectively and percentage recoveries in the range 99.65–101.43%.


Author(s):  
YASMIWAR SUSILAWATI ◽  
NYI MEKAR SAPTARINI ◽  
ZELIKA MEGA RAMADHANIA ◽  
ELI HALIMAH ◽  
NAILAH NURJIHAN ULFAH

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%.


2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 42-48
Author(s):  
P. J. Patel ◽  
◽  
D. A Shah ◽  
F. A. Mehta ◽  
U. K. Chhalotiya

A simple, sensitive and precise high performance thin layer chromatographic (HPTLC)method has been developed for the estimation of ondansetron (OND) and ranitidine (RAN) in combination. The method was employed on thin layer chromatography (TLC) and aluminium plates were precoated with silica gel 60 F254 as the stationary phase, while the solvent system was methanol. The Rf values were observed to be 0.5 ± 0.02, and 0.3 ± 0.02 for OND and RAN, respectively. The separated spots were densitometrically analyzed in absorbance mode at 299 nm. This method was linear in the range of 25-300 ng/band for OND and 50-600 ng/band for RAN. The limits of detection for OND and RAN were found to be 3.47 and 1.83 ng/band, respectively. The limits of quantification for OND and RAN were found to be 10.53 and 5.55 ng/band, respectively. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of OND and RAN in combined dosage form.


Sign in / Sign up

Export Citation Format

Share Document