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EN
A sensitive, selective, precise, and stability-indicating HPTLC method has been established for analysis of amtolmetin guacil both as the bulk drug and in a formulation. Aluminum foil-backed silica gel 60F 254 plates were used with toluene-ethyl acetate 4:6 ( υ/υ ) as mobile phase, and densitometric analysis was performed in absorbance mode at 320 nm. The method was validated for linearity, precision, accuracy, selectivity, and specificity in accordance with ICH guidelines. Amtolmetin guacil was subjected to acidic and alkaline hydrolysis, oxidation, dry heat treatment, and photo-degradation. The method was used to study the kinetics of degradation of amtolmetin guacil by acid and alkali.
EN
This paper describes a new, simple, precise, and accurate HPTLC method for quantification of (−)-epicatechin in the leaves of Cassia fistula . The leaves were separately extracted with methanol and water by both maceration and hot extraction (Soxhlet apparatus). Chromatographic separation of the drug was performed on aluminium foil silica gel 60 F 254 plates with toluene-ethyl acetate-formic acid-methanol 20:12:4:4 ( v / v ) as mobile phase. Densitometric evaluation of the separated zone was performed at 280 nm. Epicatechin in the extract was satisfactorily resolved with R F 0.22 ± 0.02. The accuracy and reliability of the method were assessed by evaluation of linearity (200–800 ng per band), precision (method precision RSD 1.42% and instrumental precision RSD 1.12%), accuracy (98.12%), and specificity in accordance with ICH guidelines.
EN
An accurate, sensitive, rapid, and precise stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of nebivolol hydrochloride and hydrochlorothiazide as the bulk drug and in tablets has been developed and validated. Optimum separation was achieved on silica gel 60 F 254 plates with ethyl acetate-methanol-acetic acid 6.5:1:0.5 ( υ/υ ) as mobile phase. Detection and quantification were performed at 280 and 270 nm for nebivolol hydrochloride and hydrochlorothiazide, respectively. The drugs get resolved with R F 0.46 ± 0.02 and 0.78 ± 0.02 for nebivolol hydrochloride and hydrochlorothiazide, respectively. The drugs were subjected to hydrolysis under acidic, basic, and neutral conditions, oxidation, heat, and photolysis as stress conditions. Peaks of degradation products were observed when the drugs were subjected to oxidative stress. Acidic conditions were also found to affect the tablet sample substantially. The degradation products resulting from stress conditions did not interfere with the drug peak. The method can be used for stability testing of these drugs during stability studies.
EN
A sensitive, selective, precise, and stability-indicating HPTLC method for quantitative analysis of quetiapine fumarate both as the bulk drug and in formulations has been established and validated. The stationary phase was silica gel and the mobile phase toluene-methanol 8:2 (v/v). This system gave compact bands for quetiapine fumarate ( R F 0.37 š 0.02). Densitometric analysis of quetiapine fumarate was performed in absorbance mode at 254 nm. There was no chromatographic interference from tablet excipients. Quetiapine fumarate was subjected to acid and alkaline hydrolysis, oxidation, and photodegradation. The drug is susceptible to all these treatments. The degradation products were well resolved from the pure drug with substantially different R F values. The method was validated for linearity, precision, accuracy, selectivity, and specificity in accordance with ICH guidelines. Because the method can effectively separate the drug from its degradation products, it can be used as a stability indicating method.
EN
A simple, precise, and accurate HPTLC method has been established for simultaneous quantification of aspirin, atorvastatin calcium and clopidogrel bisulphate in the bulk drug and in a capsule dosage form. Chromatographic separation of the drugs was performed on aluminium foil plates precoated with silica gel 60 F 254 , with toluene-methanol-formic acid 6.5:3.5:0.1 ( v / v ) as mobile phase. Densitometric evaluation of the separated zones was performed at 254 nm. The three drugs were satisfactorily resolved with R F ± SD values 0.26 ± 0.01, 0.47 ± 0.01, and 0.78 ± 0.01 for aspirin, atorvastatin calcium, and clopidogrel bisulphate, respectively. The method was validated for linearity, specificity, accuracy, precision, and robustness, in accordance with ICH guidelines. Results from recovery studies indicated acceptable recovery of the drugs from the capsule dosage form. The intra-day and inter-day relative standard deviations were in the ranges 0.17–0.73% and 0.46–1.03% for aspirin, 0.36–0.87% and 0.44–0.62% for atorvastatin calcium, and 0.25–0.69% and 0.35–0.94% for clopidogrel bisulphate. The method proved to be a rapid and cost-effective quality-control tool for routine simultaneous analysis of aspirin, atorvastatin calcium, and clopidogrel bisulphate in the bulk drug and in a capsule formulation.
EN
Eladi Gutika is a polyherbal formulation official in “Ayurvedic formulary of India” and used for dry cough and throat infection. A simple, specific and precise high-performance thin-layer chromatography (HPTLC) method has been developed for quantification of piperine and 18-β glycyrrhetinic acid in Eladi Gutika. We report the extraction and estimation of these compounds in a laboratory prepared sample of Eladi Gutika and two of its marketed formulations. The compounds were chromatographed on precoated silica gel G 60254 plates in the mobile phase comprising of toluene, ethyl acetate, and glacial acetic acid. Under the optimized chromatographic conditions, the calibration plot was found to be linear in the range of 0.2–1 g mL-1 with a correlation coefficient R2 = 0.9902 for piperine and 0.9904 for 18-β glycyrrhetinic acid. Mean recovery for piperine was 99.75% w/w and for 18-β glycyrrhetinic acid was 101.36% w/w.
EN
In this reported study, a direct high-performance thin-layer chromatographic (HPTLC) method was developed to qualitatively detect and quantitatively determine glycerol in Antarctic krill for the first time. This procedure was based on the extraction of glycerol by ultrasonic solvent extraction with anhydrous ethanol, silica-gel column chromatographic separation, HPTLC detection and quantification using methylene chloride–methanol (5:1, v/v) as the developing solvent and alkaline potassium permanganate as chromogenic agent. The content of glycerol was 1.3725 ± 0.218 mg/g in freeze-dried Antarctic krill. The structure of glycerol in the Antarctic krill was subsequently determined by gas chromatography–mass spectrometry (GC–MS) which verified the presence of the material in the krill. The HPTLC method exhibited excellent accuracy with a recovery of 90.1–103.3% and good precision with a relative standard deviation (RSD) of 1.59–4.84%. The results clearly exhibited the applicability of the proposed for quantifying glycerol in Antarctic krill.
EN
In this paper we describe a simple, precise, and accurate HPTLC method for quantification of lupeol in the bark of Mimosoups elengi (ME). The bark was extracted with hot methanol in a Soxhlet apparatus. Chromatographic separation of the extract was performed on aluminum foil plates coated with silica gel 60 F 254 as the stationary phase. The mobile phase was toluene-ethyl acetate-formic acid 12:2:1 ( υ/υ ). Densitometric evaluation of the separated zones was performed at 220 nm. The lupeol was satisfactorily resolved at R F 0.64 ± 0.02. The accuracy and reliability of the method were assessed by evaluation of linearity (1000–4000 ng per band), precision (method and instrumental precision, as RSD, 1.06 and 1.03%, respectively), accuracy (97.28 ± 0.89), and specificity in accordance with ICH guidelines.
9
Content available remote Densitometric HPTLC and HPLC analysis of phenolic acids from Aquilegia vulgaris
100%
EN
Densitometric HPTLC and HPLC have been used for quantification of p -coumaric and protocatechuic acids in an ethereal fraction from a methanolic extract of Aquilegia vulgaris L. HPLC analysis was performed on an RP-18 column with methanol-water-formic acid 25:75:0.5 ( υ/υ ) as mobile phase. Thin layer chromatography was performed on Si60 F 254 HPTLC plates with mixtures of heptane, dichloromethane, diisopropyl ether, formic acid, and water as mobile phases. Satisfactory separation of the phenolic acids was achieved by use of the multiple gradient development technique. The quantities of p -coumaric and protocatechuic acids determined by HPLC were 0.374 and 2.283 mg g -1 dry plant material, respectively; HPTLC results were somewhat higher - 0.396 and 2.584 mg g -1 , respectively. The precision of both methods, expressed as relative standard deviation, was satisfactory. The methods are useful for quality control of Aquilegia vulgaris extracts.
EN
Methods based on RP-HPLC and HPTLC with UV detection for rapid quantitative determination of marker component in Enicostemma hyssopifolium, swertisin are described. The recovery of the compound was between 96.3–101.5% by HPTLC method and 98.9–100.2% by HPLC assay. The relative standard deviations ranged between 1.53–1.81 (intra-day) and 1.33–1.96 (inter-day) for HPTLC and 0.60–1.11 (intra-day) and 0.80–1.20 (inter-day) for HPLC. The methods were used for routine analysis of swertisin in the aerial parts of the plant. HPTLC method was found to be more economic and less time consuming than HPLC. Reproducibility and recovery in HPLC method were better than that in HPTLC method.
11
89%
EN
The aim of this work was isolation from water and the determination of PAHs, which are the most dangerous for human health. It was done by the use of solid phase extraction and planar chromatography with densitometric detection. Planar separations were performed using HPTLC impregnated with caffeine. Standards and samples were applied to the chromatographic plates by Nanomat, and then developed with dichloromethane in horizontal chamber. Limits of detection of six PAHs were evaluated as well as their quantitation by means of a densitometer was perfornled.
PL
W pracy wydzielano i oznaczano w wybranych wodach sześć wielopierścieniowych węglowodorów aromatycznych (WWA), które są najbardziej niebezpieczne dla zdrowia ludzkiego. W tym celu wykorzystano ekstrakcję do fazy stałej oraz chromatografię planarną z detekcją densytometryczną. Rozdziały techniką chromatografii planarnej przeprowadzono stosując płytki HPTLC z warstwą żelu krzemionkowego impregnowaną kofeiną. Wzorce i próbki nanoszono na płytki chromatograficzne za pomocą aplikatora i rozwijano dichlorometanem w komorze poziomej. Wyznaczono granice wykrywalności sześciu WWA oraz przeprowadzono ich analizę ilościową w wodzie.
12
Content available remote Determination of some psychotropic drugs in human plasma by HPTLC
88%
EN
Psychotropic drugs: desipramine, olanzapine and mitrazapine were chromatographed on cyanopropyl-silica and Diol-silica thin layers using various nonaqueous and aqueous eluents.The best results were obtained with addition of ammonia to nonaqueous eluent on both adsorbents. On the basis of the optimization, systems for extraction from human plasma and quantitative determination of investigated drugs were selected.RP18 encaped SPE columns conditioned and pre-eluted with acetonitrile:water:ammonium buffer at pH 8.6 (5:5:2) and eluted with methanol:water (9:1) containing 2% acetic acid were used for sample preparation with high recoveries of all investigated drugs. Diol and CN plates with mixture of 15% methanol in diisopropyl ether + 1% ammonia were used for quantitative analysis by a calibration curve method.
13
88%
EN
A simple, selective, precise, and stability-indicating high-performance thin layer chromatographic (HPTLC) method has been established and validated for the analysis of idebenone in bulk drug and formulations. The compounds were analyzed on aluminum-backed silica gel 60 F254 plates with petroleum ether-methanol (4:1, υ/υ) as mobile phase. Densitometric analysis of idebenone was performed at 282 nm. Regression analysis data for the calibration plots were indicative of good linear relationship between response and concentration over the range of 200–600 ng per spot. The correlation coefficient (r2) was 0.989 ± 0.002. The values of slope and intercept of the calibration plots were 2.386 ± 0.0435 and 577.733 ± 19.545, respectively. The method was validated for precision, accuracy, robustness, and ruggedness. The limits of detection and quantification were 14.642 and 44.369 ng, respectively. Idebenone was subjected to acid, base, peroxide, and sunlight degradation. In stability tests, the drug was susceptible to acid and basic hydrolysis, oxidation, and photodegradation.
EN
A sensitive, accurate, and robust high-performance thin-layer chromatographic (HPTLC) method has been established for simultaneous analysis of wedelolactone (WED) and asiaticoside (ASI) in Eclipta alba and Centella asiatica Linn., respectively. Chromatography was performed on silica gel with toluene-acetone-methanol-formic acid 3.0:2.0:2.0:0.05 ( υ/υ ) as mobile phase. Densitometric scanning at 317 nm for WED and at 530 nm, after derivatisation with 10% methanolic sulphuric acid, for ASI was used. The method was validated in accordance with the guidelines of the International Conference on Harmonization (ICH). R F values of 0.26 and 0.75 were obtained for ASI and WED, respectively. The linear ranges were 50–250 and 150–550 ng per band for WED and ASI, respectively, with good correlation coefficients ( r 2 = 0.999 and 0.9989, respectively). Accuracy was 99.29% and 99.45% for WED and ASI, respectively. The method was found to be precise, robust, and suitable for routine quality-control analysis of plant extracts and polyherbal formulations.
EN
High-performance thin-layer chromatography (HPLTC)–densitometry methods are described for the analysis of the anti(retro)virals dolutegravir (D), lamivudine (L), and tenofovir disoproxil fumarate (TDF) in a pharmaceutical tablet product. To the best of our knowledge, no previous quantitative planar chromatography method has been reported in the literature for this combination formulation. The method for L was transferred from a thin-layer chromatography (TLC) screening method published in the Global Pharma Health Fund (GPHF) Minilab Manual designed for identification of counterfeit and substandard drug products using a model process published earlier. D and TDF are not included in the list of drugs for which TLC screening methods are published for the Minilab, but HPTLC–densitometry procedures were developed for them using the transfer process guidelines. L was analyzed simultaneously with TDF on Merck Premium Purity silica gel 60 F plates using the mobile phase ethyl acetate–methanol–acetone–concentrated ammonium hydroxide (30:7:3:1) and densitometric scanning at 254 nm. D was analyzed on a second plate by scanning at 366 nm after chromatography with the chloroform–methanol–formic acid (32:8:2) mobile phase. Data for all three drugs are shown to meet the requirements of the model transfer process for calibration curve r values, assay of tablets relative to their label values, peak purity/peak identity tests, and validation by standard addition analysis of samples spiked at 50%, 100%, and 150% of the label value of active ingredients. A TLC screening method for TDF in the combination product was developed and published online with open access.
16
Content available remote Biennial review of planar chromatography: 2011–2013
88%
Open Chemistry
|
2014
|
tom 12
|
nr 4
427-452
EN
The most important advances in planar chromatography published between November 1, 2011 and November 1, 2013 are reviewed in this paper. Included are an introduction to the current status of the field; student experiments, books, and reviews; theory and fundamental studies; apparatus and techniques for sample preparation and TLC separations (sample application and plate development with the mobile phase); detection and identification of separated zones (chemical and biological detection, TLC/mass spectrometry, and TLC coupled with other spectrometric methods); techniques and instruments for quantitative analysis; preparative layer chromatography; and thin layer radiochromatography. Numerous applications to a great number of compound types and sample matrices are presented in all sections of the review.
EN
A simple, selective, precise, and stability-indicating high-performance thinlayer chromatographic method for analysis of sitagliptin phosphate both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed high-performance thin-layer chromatography (HPTLC) aluminium plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of methanol-water-triethylamine (8:2:0.05 v/v). The system was found to give compact spot for sitagliptin phosphate (Rf value of 0.55 ± 0.03). Densitometric analysis of sitagliptin phosphate was carried out in the absorbance mode at 267 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.998±0.0015 with respect to peak area in the concentration range 1000–6000 ng per spot. The mean value ± SD of slope and intercept was 0.723 ± 0.043 and 17.24 ± 18.78 with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 85.80 and 265.42 ng per spot, respectively. Sitagliptin phosphate was subjected to acid and alkali hydrolysis, oxidation, and photo and thermal degradation. The drug undergoes degradation under acidic, basic, and oxidative conditions. This indicates that the drug is susceptible to acid and base, and oxidation. The degraded product was well resolved from the pure drug with significantly different RF value. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of sitagliptin phosphate in bulk drug and pharmaceutical formulation.
EN
A new, simple, accurate, and precise high-performance thin-layer chromatographic (HPTLC) method has been established for simultaneous analysis of eprosartan and hydrochlorothiazide in tablet formulations. Standard and sample solutions of eprosartan and hydrochlorothiazide were applied to precoated silica gel G 60 F 254 HPTLC plates and the plates were developed with benzene-methanol-formic acid 7:3:0.1 ( υ/υ ) as mobile phase. Detection and evaluation of chromatograms was performed densitometrically at 272 nm. The retention factors of eprosartan and hydrochlorothiazide were 0.76 and 0.57, respectively. The linear range was 4.8–43.2 μg per spot for eprosartan and 0.15–1.35 μg per spot for hydrochlorothiazide; the correlation coefficients, r , were 0.998 and 0.999, respectively. The method was validated and successfully used for analysis of the drugs in tablets.
EN
Gymnemic acid (GA) is one of the phytoconstituents present in Gymnema sylvestre. Estimation of GA was carried out first time from microencapsulated polyherbal formulation. Microencapsulated polyherbal formulations (F1 and F2) contain various plant extracts; hence, proper resolution of GA peak in high-performance thin-layer liquid chromatography (HPTLC) analysis of F1 and F2 is the problem. Hence, HPTLC analysis method for F1 and F2 is developed and validated for quantitative determination of GA. HPTLC analysis of F1 and F2 was carried out using TLC aluminum plates precoated with silica gel 60F254 eluted with chloroform-methanol-water (6.5 mL + 4.5 mL + 1.0 mL), and densitometric analysis was carried out at 580 nm. Complete validation was performed using standard methods. This HPTLC method was found to be reproducible, accurate, and can detect GA at microgram level. The new optimized mobile phase gave good resolution of GA peak for its proper quantification in microencapsulated polyherbal formulation.
EN
This paper describes a simple, precise, and accurate HPTLC method for simultaneous quantification of sennoside A, sennoside B, and kaempferol in Cassia fistula whole plant extract. Chromatographic separation of the sample extract was performed on aluminium foil plates coated with silica gel 60 F 254 as stationary phase. The mobile phase was toluene-ethyl acetate-methanol-formic acid 8:10:5:2 ( υ/υ ). Densitometric evaluation of the separated bands was performed at 270 nm. Sennosides A and B and kaempferol were satisfactorily resolved at R F 0.22 ± 0.05, 0.19 ± 0.05, and 0.81 ± 0.05, respectively. Recovery of sennosides A and B and kaempferol from Cassia fistula extract was 98.03, 98.74, and 99.08%, respectively. The method was validated for specificity, accuracy, linearity (100–400 ng per band), and precision (instrument precision in the range 1.03–1.33 and method precision in the range of 1.31–1.75) in accordance with ICH guidelines.
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