Wyniki wyszukiwania - Biblioteka Nauki

1

Application of a stability-indicating HPTLC method for quantitative analysis of amtolmetin guacil in a pharmaceutical dosage form

100%

Bhusari V. K. , Mahadik M. V. , Dhaneshwar S. R.

Acta Chromatographica

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2009

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tom Vol. 21, no. 2

299--317

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.

2

Simultaneous HPTLC analysis of aspirin, atorvastatin calcium and clopidogrel bisulphate in the bulk drug and in capsules

100%

Londhe S. V. , Mulgund S. V. , Deshmukh R. S. , Jain K. S.

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2010

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tom Vol. 22, no. 2

297--305

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.

3

Validated HPTLC method for quantification of epicatechin in extracts of leaves of Cassia fistula Linn.

100%

Nagore D. H. , Ghosh V. K. , Patil M. J. , Wahile A. M.

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2010

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tom Vol. 22, no. 2

259--265

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.

4

Stability-indicating HPTLC method for quantitation of quetiapine fumarate in the pharmaceutical dosage form

100%

Dhaneshwar S. R. , Patre N. G. , Mahadik M. V.

Acta Chromatographica

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2009

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tom Vol. 21, no. 1

83-93

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.

5

Development and validation of a stability-indicating HPTLC method for analysis of nebivolol hydrochloride and hydrochlorothiazide in the bulk material and in pharmaceutical dosage forms

100%

Damle M. C. , Topagi K. S. , Bothara K. G.

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2010

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tom Vol. 22, no. 3

433--443

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.

6

Quantification of piperine and 18-β glycyrrhetinic acid in herbal formulation “Eladi Gutika”

100%

Rode S. , Bhujbal P. , Sandhya P.

Acta Chromatographica

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2013

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tom Vol. 25, no. 1

135--146

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.

7

Quantitative determination of glycerol in antarctic krill (Euphausia superba Dana) by high-performance thin-layer chromatography

100%

Han X. , Liu D.

Acta Chromatographica

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2018

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tom Vol. 30, no. 4

274--277

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.

8

Wykorzystanie chromatografii HPTLC w analizie produktów pszczelich

89%

Miłek M.

Przemysł Spożywczy

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2023

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tom T. 77, nr 9

15--19

PL

Wysokosprawna chromatografia cienkowarstwowa (HPTLC) jest techniką chromatograficzną często wykorzystywaną w analizie żywności. Może być stosowana do analiz jakościowych (np. profilowanie składu próbki) i ilościowych, a szczególnie przydatna jest w analizie porównawczej wielu próbek rozdzielanych jednocześnie na płytce. Wśród wielu zastosowań tej techniki analitycznej znajduje się ocena jakości produktów pszczelich, zwłaszcza miodu, propolisu i pyłku pszczelego, ale także mniej popularnych produktów, jak pierzga, mleczko pszczele czy czerw trutowy. Wśród najczęściej badanych tą metodą parametrów są: profil polifenolowy, cukrowy czy aminokwasowy, istnieje też możliwość oznaczania konkretnych związków, odpowiedzialnych za bioaktywność produktów pszczelich lub stanowiących substancje niepożądane (np. HMF). Zaletami metody HPTLC są jej prostota, możliwość analizy nawet kilkunastu próbek jednocześnie, brak konieczności specjalnego przygotowania próbki oraz stosunkowo niewielki koszt pojedynczej analizy.

EN

High-performance thin-layer chromatography (HPTLC) is a chromatographic technique that is increasingly used in food analysis. Suitable for qualitative (sample composition profiling) and quantitative analyses, it is particularly useful in the comparative analysis of multiple samples separated simultaneously on the plate. Among the many applications is the assessment of the quality of bee products, especially honey, propolis and bee pollen, but also less popular products such as bee bread, royal jelly or drone brood. Among the parameters most often tested with this method is the polyphenol, sugar or amino acid profile, it is also possible to determine specific compounds responsible for the bioactivity of bee products or undesirable substances (e.g. HMF). The advantages of the HPTLC method are its simplicity, the ability to analyze multiple samples simultaneously, no need for special sample preparation and the relatively low cost of a single analysis.

9

Development and validation of HPTLC method for estimation of gymnemic acid in microencapsulated antidiabetic polyherbal formulations

88%

Patil A. N. , Nirmal S. A. , Chavan A. K.

Acta Chromatographica

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2013

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tom Vol. 25, no. 4

601--612

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.

10

Simultaneous analysis of eprosartan and hydrochlorothiazide in tablets by high-performance thin-layer chromatography with ultraviolet absorption densitometry

88%

Patel H. U. , Suhagia B. N. , Patel C. N.

Acta Chromatographica

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2009

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tom Vol. 21, no. 2

319--326

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.

11

Determination of some psychotropic drugs in human plasma by HPTLC

88%

Wróblewski K. , Petruczynik A. , Waksmundzka-Hajnos M.

Acta Chromatographica

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2014

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tom Vol. 26, no. 2

297--307

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.

12

Development and validation of a stability-indicating HPTLC assay method for idebenone

88%

Rathi A. A. , Dhamecha D. L. , Dehghan M. H. G. , Saifee M. , Wakte P. S. , Shelke S. D. , Dongre S. H.

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2011

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tom Vol. 23, no. 2

281--294

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.

13

Development and validation of a densitometric HPTLC method for simultaneous analysis of wedelolactone and asiaticoside in a polyherbal formulation

88%

Sathiyanarayanan L. , Paradkar A. R. , Mahadik K. R.

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2010

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tom Vol. 22, no. 4

651--663

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.

14

Development of quantitative HPTLC methods for dolutegravir, lamivudine, and tenofovir disproxil fumarate in a combination pharmaceutical product using a model process published earlier for transfer of minilab TLC screening methods to HPTLC-densitometry

88%

Gu Y. , Zeng B. , Sherma J.

Acta Chromatographica

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2020

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tom Vol. 32, no. 3

199--202

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.

15

Biennial review of planar chromatography: 2011–2013

88%

Sherma J.

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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.

16

Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of sitagliptin phosphate monohydrate in bulk and in pharmaceutical formulation

88%

Jain P. S. , Chaudhari A. J. , Surana S. J.

Acta Chromatographica

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2014

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tom Vol. 26, no. 2

309--319

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.

17

Validated HPTLC method for simultaneous quantification of sennoside A, sennoside B, and kaempferol in Cassia fistula Linn.

88%

Bhope S. G. , Kuber V. V. , Nagore D. H.

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2010

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tom Vol. 22, no. 3

481--489

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.

18

Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of repaglinide in bulk and in pharmaceutical formulation

88%

Jain P. S. , Patel M. K. , Surana S. J.

Acta Chromatographica

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2013

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tom Vol. 25, no. 3

531--544

EN

A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis of repaglinide both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed high-performance thin-layer chromatography (HPTLC) aluminum plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of chloroform-methanol-ammonia (4.5:0.8:0.05, v/v). The system was found to give compact spot for repaglinide (RF value of 0.55 ± 0.03). Densitometric analysis of repaglinide was carried out in the absorbance mode at 288 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 600–1600 ng per spot. The mean value ± SD of slope and intercept were 3.38 ± 1.47 and 986.9 ± 108.78, with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 22.64 and 68.84 ng per spot, respectively. Repaglinide was subjected to acid and alkali hydrolysis, oxidation, and thermal degradation. The drug undergoes degradation under acidic and basic conditions. This indicates that the drug is susceptible to acid and base. 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 repaglinide in bulk drug and pharmaceutical formulation.

19

Determination of ampicillin and amoxicillin by high-performance thin-layer chromatography

88%

Ghoulipour V. , Shokri M. , Waqif-Husain S.

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2011

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tom Vol. 23, no. 3

483--498

EN

A simple and fast high-performance thin-layer chromatographic method has been developed for the simultaneous determination of ampicillin and amoxicillin. Titanium(IV) silicate (a synthetic inorganic ion-exchanger)-coated thin-layer chromatography (TLC) plates were used to separate them, employing a mixture of K2HPO4 (0.1 M) + KH2PO4 (0.1 M), 1:1 (υ/υ), as mobile phase. The development time was 18 min. The plates were sprayed with fresh 1% solution of ninhydrin in ethanol. The developed method enables highly contrasted chromatograms with red purple spots in white background. Densitometric measurements were made at wavelength 546 nm using Camag TLC Scanner-3. The ampicillin and amoxicillin recovery of the total procedure were equal to 99.99 and 100.43, respectively. The procedure is quantitatively characterized. Linearities were r2 > 0.9958 and 0.9954 for ampicillin and amoxicillin, respectively, and the relative standard deviations were <0.89 and 0.61, respectively. The limits of detection were 2.9 and 1.5 ng per spot and the limits of quantification were 14.5 and 7.5 ng per spot, respectively. The method is rapid, selective, precise, and accurate and thus can be used for the routine analysis of pharmaceutical preparations in quality control laboratories of the pharmaceutical industry. The method is successfully applied for the determination of ampicillin and amoxicillin in human blood plasma and urine.

20

HPTLc method development and validation for analysis of risperidone in formulations, and in-vitro release study

75%

Patel R. B. , Patel B. G. , Patel M. R. , Bhatt K. K.

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2010

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tom Vol. 22, no. 4

549--567

EN

A new, simple, and rapid high-performance thin-layer chromatographic method has been established for quantitative analysis of risperidone. Chromatography was performed on silica gel 60 F 254 plates with methanol-ethyl acetate 8.0:2.0 ( v / v ) as mobile phase. Risperidone was quantified by densitometric analysis at 285 nm. The method gave compact bands for the drug ( R F 0.34 ± 0.01). Linear regression analysis of calibration data revealed a good linear relationship ( r 2 = 0.9996) between response and amount of risperidone in the range 100–600 ng per band. The method was validated for precision, recovery, repeatability, linearity, specificity, and robustness in accordance with ICH guidelines. The minimum detectable amount was 22.44 ng per band and the limit of quantification was 68.01 ng per band. Statistical analysis of the results showed the method enabled precise, accurate, reproducible, and selective analysis of risperidone. The method was successfully used for estimation of the equilibrium solubility of risperidone, and for quantification of risperidone as the bulk drug in a commercially available preparation, in in-house-developed mucoadhesive microemulsion formulations, and in solution.