Thin-Layer Chromatography-Densitometric Analysis of -Mangostin Content in Garcinia mangostana Fruit Rind Extracts

Abstract The fruit rinds of mangosteen (Garcinia mangostana Linn.) have long been used as traditional medicines for treatment of skin infections, wounds, and diarrhea. A simple thin-layer chromatography (TLC)-densitometric method has been developed for the simultaneous quantification of -mangostin in the extracts from unripe and ripe fruit rinds of G. mangostana. It was found in the ranges of 10.48 0.83 and 16.65 0.38 (w/w) in the dried unripe and ripe fruit rinds, respectively. The method was validated for linearity, precision, accuracy, limit of detection (LOD), and limit of quantitation (LOQ). The linearity was found over the range of 100500 ng/spot with regression coefficient 0.999. Intraday and interday precision studies showed the relative standard deviation was <2. Accuracy of the method was determined by a recovery study conducted at 3 different levels, and the average recovery was 99.49. The LOD and LOQ were 40 and 100 ng, respectively. The proposed TLC-densitometric method was found to be simple, precise, specific, sensitive, and accurate. This method can be used for routine quality control of raw material of G. mangostana fruit rind, extract, and its products. It also can be applied in quantifying this marker compound in other drugs.

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

Journal of AOAC International ◽

10.1093/jaoac/89.1.1 ◽

2006 ◽

Vol 89 (1) ◽

pp. 1-7 ◽

Cited By ~ 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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Thin-Layer Chromatography-Densitometric Measurements for Determination of N-(Hydroxymethyl)nicotinamide in Tablets and Stability Evaluation in Solutions

Journal of AOAC International ◽

10.1093/jaoac/91.5.1186 ◽

2008 ◽

Vol 91 (5) ◽

pp. 1186-1190 ◽

Cited By ~ 3

Author(s):

Urszula Hubicka ◽

Jan Krzek ◽

Justyna uka

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Limit Of Detection ◽

Good Precision ◽

First Order ◽

Kinetic And Thermodynamic Parameters ◽

Relative Standard ◽

Basic Solutions ◽

Layer Chromatography

Abstract A thin-layer chromatography (TLC)-densitometric method was developed to determine N-(hydroxymethyl)nicotinamide in tablets and basic solutions along with nicotinic acid. Analysis was performed on silica gel F254 plates using chloroformethanol (2 + 3, v/v) mobile phase. The densitometric observations were made at 260 nm. The results showed good precision and accuracy; relative standard deviation was 2.37, and recovery ranged from 97.60 to 100.82. The limit of detection was 0.1 g/spot, while the linearity range was from 0.2 to 1.75 g/spot. Applicability of the newly developed method was tested for determination of N-(hydroxymethyl)nicotinamide in the preparation Cholamid. Densitometric measurements were used to evaluate stability of N-(hydroxymethyl)nicotinamide in basic solutions. It was found that decomposition corresponded to first-order reaction kinetics. The computed kinetic and thermodynamic parameters at 30C were as follows: k 0.00675/min, t0,5 1.71 h, t0,1 0.26 h, and Ea 44.75 kJ/mol.

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Simultaneous HPTLC Estimation of Simvastatin and Ezetimibe in Tablet Dosage Form

E-Journal of Chemistry ◽

10.1155/2010/845862 ◽

2010 ◽

Vol 7 (4) ◽

pp. 1206-1211 ◽

Cited By ~ 2

Author(s):

Bhupendra Shrestha ◽

B. Stephenrathinaraj ◽

Sita Sharan Patel ◽

N. K. Verma ◽

R. Mazumder

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

High Performance ◽

Dosage Form ◽

Limit Of Detection ◽

Percent Recovery ◽

Limit Of Quantitation ◽

The Mean ◽

Tablet Dosage ◽

Layer Chromatography

A method enabling the precise and quick simultaneous analysis of simvastatin and ezetimibe in tablet formulation by high performance thin layer chromatography has been presented. Samples of simvastatin and ezetimibe in organic solvents were separated on a plate coated with silica gel 60 F-254 and the chromatograms were developed using a mixture of chloroform and methanol (9.5: 0.5 %v/v). The method has a linearity range of 40-280 ng.mL-1for both the drugs when scanned at 254 nm. The limit of detection and limit of quantitation was found to be 30 and 100 ng.band-1respectively, for both the drugs. The mean percent recovery was found to be 100.65 and 101.55 for simvastatin and ezetimibe. The intra-day and inter-day precision studies were carried out with mean RSD of 0.88 and 1.27 for ezetimibe and 1.35 and 1.50 for simvastatin.

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Validated HPTLC Method for the Determination of Nintedanib in Bulk Drug

Proceedings ◽

10.3390/ecsoc-22-05675 ◽

2018 ◽

Vol 9 (1) ◽

pp. 22

Author(s):

Debanchal Dutta ◽

Soumyajit Das ◽

Manik Ghosh

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Kinase Inhibitor ◽

Limit Of Detection ◽

Calibration Plot ◽

Technical Requirements ◽

Limit Of Quantitation ◽

Bulk Drug ◽

Layer Chromatography ◽

Hptlc Method

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%.

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OPTIMIZATION OF THIN LAYER CHROMATOGRAPHY METHODS FOR SEPARATION AND IDENTIFICATION OF ANTIDEPRESSANTS IN THEIR MIXTURE

Medicinos teorija ir praktika ◽

10.15591/mtp.2015.002 ◽

2014 ◽

Vol 21 (1) ◽

pp. 11-15

Author(s):

Daiva Kazlauskienė ◽

Guoda Kiliuvienė ◽

Palma Nenortienė ◽

Giedrė Kasparavičienė ◽

Ieva Matukaitytė

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Solvent System ◽

Ammonia Solution ◽

Relative Standard ◽

Rf Values ◽

Solvent Systems ◽

Paroxetine Hydrochloride ◽

Fluvoxamine Maleate ◽

Layer Chromatography

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly

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

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2016v8i12.14953 ◽

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

Objective: 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.Methods: The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F254 using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.Results: This system was found to have a compact spot of 10-gingerol at RF value of 0.57±0.03. For the proposed procedure, linearity (r2 = 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.Conclusion: 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.

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Quantification of Eugenol, Luteolin, Ursolic Acid, and Oleanolic Acid in Black (Krishna Tulasi) and Green (Sri Tulasi) Varieties of Ocimum sanctum Linn. Using High-Performance Thin-Layer Chromatography

Journal of AOAC International ◽

10.1093/jaoac/89.6.1467 ◽

2006 ◽

Vol 89 (6) ◽

pp. 1467-1474 ◽

Cited By ~ 23

Author(s):

Sheetal Anandjiwala ◽

Jyoti Kalola ◽

Mandapati Rajani

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Ursolic Acid ◽

Oleanolic Acid ◽

High Performance ◽

Ocimum Sanctum ◽

Relative Standard ◽

Recovery Study ◽

Acid Reagent ◽

Layer Chromatography

Abstract Ocimum sanctum (family Lamiaceae) is a reputed drug of Ayurveda, commonly known as Tulasi. Inthe present work, we quantified 4 marker compounds, viz., eugenol, luteolin, ursolic acid, and oleanolic acid, from the leaf of green and black varieties of O. sanctum using high-performance thin-layer chromatography (HPTLC) with densitometry. The methods were found to be precise, with relative standard deviation (RSD) values for intraday analyses in the range of 0.52 to 0.91%, 0.77 to 1.29%, 0.11 to 0.16%, and 0.34 to 0.42% and for interday analyses in the range of 0.73 to 0.96%, 1.02 to 2.08%, 0.11 to 0.12%, and 0.39 to 0.64% for different concentrations of eugenol, luteolin, ursolic acid, and oleanolic acid, respectively. Instrumental RSD values were 0.24, 0.39, 0.21, and 0.18% for eugenol, luteolin, ursolic acid, and oleanolic acid, respectively. Accuracy of the methods was checked by conducting a recovery study at 3 different levels for the 4 compounds, and the average recoveries were found to be 99.73, 99.3, 100.58, and 100.57%, respectively. Eugenol content ranged from 0.175 to 0.362% (w/w) and luteolin from 0.019 to 0.046% (w/w) in the samples analyzed. Green variety was found to contain higher amounts of ursolic acid [0.478 and 0.348% (w/w), from Sources 1 and 2, respectively] than the black variety [0.252 and 0.264% (w/w) from Sources 1 and 2, respectively]. Black variety had 0.174 and 0.218% (w/w) of oleanolic acid from Sources 1 and 2, respectively, while it was not detected in the green variety. Ursolic acid and oleanolic acid ran at the same Rf value and could not be resolved in several solvent systems tried. However, we observed that only ursolic acid gave yellow fluorescence under 366 nm ultraviolet light after derivatization with anisaldehydesulfuric acid reagent. The HPTLC-densitometry methods for the quantification of the 4 markers in O. sanctum leaf will have the applicability in quality control.

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

Journal of AOAC International ◽

10.1093/jaoac/77.4.939 ◽

1994 ◽

Vol 77 (4) ◽

pp. 939-941 ◽

Cited By ~ 3

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.

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High-Performance Thin-Layer Chromatography Densitometric Method for Simultaneous Quantitation of Phyllanthin, Hypophyllanthin, Gallic Acid, and Ellagic Acid in Phyllanthus amarus

Journal of AOAC International ◽

10.1093/jaoac/89.3.619 ◽

2006 ◽

Vol 89 (3) ◽

pp. 619-623 ◽

Cited By ~ 29

Author(s):

Kamlesh Dhalwal ◽

Yogesh S Biradar ◽

Mandapati Rajani

Keyword(s):

Thin Layer ◽

Gallic Acid ◽

Thin Layer Chromatography ◽

Ellagic Acid ◽

High Performance ◽

Raw Material ◽

Phyllanthus Amarus ◽

Whole Plant ◽

Recovery Study ◽

Layer Chromatography

Abstract Whole plant of Phyllanthus amarus Linn. is a reputed drug of the Indian systems of medicine that is used as hepatoprotective agent. A simple high-performance thin-layer chromatography (HPTLC) densitometric method has been developed for the simultaneous quantitation of phyllanthin, hypophyllanthin, gallic acid, and ellagic acid in the whole plant of P. amarus. They were found at levels of 0.37, 1.16, 0.36, and 0.17% (w/w), respectively. The method was validated for precision, repeatability, and accuracy. Instrumental precision was found to be 0.54, 0.93, 0.08, and 0.78% (coefficient of variation, CV); repeatability of the method was 1.01, 0.79, 0.98, and 1.06% (CV) for phyllanthin, hypophyllanthin, gallic acid, and ellagic acid, respectively. Accuracy of the method was determined by a recovery study conducted at 3 different levels, and the average recovery was found to be 99.09% for phyllanthin, 99.27% for hypophyllanthin, 98.69% for gallic acid, and 100.49% for ellagic acid. The proposed HPTLC method was found to be simple, precise, specific, sensitive, and accurate and can be used for routine quality control of raw material of P. amarus and formulations containing P. amarus. It also has the applicability in quantitating any of these marker compounds in other drugs.

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

Molecules ◽

10.3390/molecules24050938 ◽

2019 ◽

Vol 24 (5) ◽

pp. 938 ◽

Cited By ~ 3

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.

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