Robustness evaluation of the chromatographic method for the quantitation of lumefantrine using Youden's test

César, Isabela Costa; Pianetti, Gérson Antônio

doi:10.1590/s1984-82502009000200007

Cited by 42 publications

(23 citation statements)

References 9 publications

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“…To evaluate the effect of each variation on the fluconazole assay the following equation was used [15].…”

Section: Validation Of Bioassay Methodsmentioning

confidence: 99%

Stability Study of Fluconazole Applying Validated Bioassay and Stability-Indicating LC Methods

Corrêa¹

2011

J Anal Bioanal Tech

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Chemical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, understanding the factors that change the stability of pharmaceuticals and identifying ways to guarantee their stability are important. In this work stability-indicating Liquid Chromatographic (LC) and bioassay methods were validated and employed in the fluconazole stability studies. The correlation of sample results from both methods was evaluated. Fluconazole raw material stability was investigated in aqueous, acid (0.1 M HCl), alkaline (0.1 M NaOH) and oxidative (3% v/v H 2 O 2 ) reflux for 6 hours, by LC method. Fluconazole capsules were exposed to UVC (254 nm, 66 and 180 days), climatic chamber (40°C, 75% RH, 90 days) and oven (60°C, 60 days), these samples were analyzed by LC and bioassay methods It was found that the drug is degraded (10% decrease) with arising of a possible degradation product in an oxidative medium and UVC exposure, in all the others conditions fluconazole remained chemically stable (higher than 98%) when analyzed by LC. However when the capsules stressed samples were evaluated through bioassay very low antifungal activity was found (about 30%). Fluconazole showed to be an unstable drug and it indicates that special care must be taken during the handling, storage and quality control using appropriated methods to analyze this therapeutic agent. This work suggests monitoring the fluconazole stability by bioassay and the stability-indicating LC methods. The aims of this study were verifying the drug stability under stress conditions and quantify it by validated bioassay and Liquid Chromatographic (LC) stability-indicating methods. Material and Methods ChemicalsFluconazole chemical reference (assigned purity of 100%) was obtained from Sigma Aldrich, fluconazole raw material was kindly donated by EMS (Campinas, Brazil). It was standardized against fluconazole chemical reference. Capsules were purchased from local markers with label of 150 mg of drug.Methanol LC grade was purchased from Tedia (Fairfield, USA). Ultrapurified water was prepared in-house by using Direct-Q® water system (Millipore Corporation, Billerica, USA). Prior to use, mobile phase solvents were degassed in an ultrasonic bath for 30 min. Sodium hydroxide, hydrochloric acid, and hydrogen peroxide (reagent grade) were purchased from Merck (Darmstadt, Germany). Purified water (<18S) was used to prepare the mobile phase, the sample and the standard solutions. Solvents were filtered through a 0.45 µm membrane filter. ApparatusLiquid Chromatography apparatus (Waters Corporation, Milford, MA, USA), equipped with a Waters 1525 binary pump, a Rheodyne Breeze 7725i manual injector, a Waters 2487 UV-VIS wavelength detector was used. In addition a Liquid Chromatography apparatus Shimadzu® CLASS-VP, with PDA detector (Shimadzu Corporate, Japan) was employed. HPLC analysis was conducted by using a RP C18 column (Symmetry Waters, Milford, MA, USA), with 5 µm particle size, 4.6 mm x 250 mm.Oven (FABBE® Ltda), climatic cham...

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“…To evaluate the effect of each variation on the fluconazole assay the following equation was used [15].…”

Section: Validation Of Bioassay Methodsmentioning

confidence: 99%

Stability Study of Fluconazole Applying Validated Bioassay and Stability-Indicating LC Methods

Corrêa¹

2011

J Anal Bioanal Tech

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“…These seven factors were combined in eight random chromatographic experiments (nominal condition + seven variants) performed with a PQ concentration of 500ng.mL -1 (corresponding to an intermediate point along the standard analytical curve) [27][28][29] . The limits of detection (LOD) and quantification (LOQ) were obtained from three calibration curves using the following equations: LOQ = DPa (standard deviation of intercept Y) × 10/IC (curve slope) and LOD = DPa × 3/IC 20,21 .…”

Section: Validationmentioning

confidence: 99%

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma

Carmo

Borborema

Ribeiro

et al. 2017

Rev. Soc. Bras. Med. Trop.

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Introduction: Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. Methods: After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min

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“…La evaluación periódica de residuos de plaguicidas requirió la implementación y verificación de la Norma EN15662, mediante el cálculo de cifras analíticas de mérito a partir de la recta de calibración, análisis de exactitud y el test de robustez, ampliamente documentado de Youden-Steiner (22,23), para el análisis simultáneo de residuos de plaguicidas organoclorados y organofosforados, por GC-µECD, en muestras de tomates comercializado en una tienda orgánica, un Fruver (comercializador de verduras, frutas y hortalizas frescas) y catorce supermercados, para un total de 16 puntos de muestreo en el municipio de Armenia. El análisis se realizó de forma periódica durante seis meses.…”

Section: Metodologíaunclassified

RESIDUOS DE PLAGUICIDAS EN TOMATE (Solanum lycopersicum) COMERCIALIZADO EN ARMENIA, COLOMBIA

Ríos

Vida

Montes

et al. 2017

Vitae

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Background: Tomato variety "chonto" (Solanum lycopersicum) is a common ingredient in Colombian cuisine. This fruit is commonly attacked for pests that generates losses higher than 30 %. The profuse crop dusting produces a risk for the consumers, for that reason The Colombian Agriculture Institute (ICA) limit the use of agrochemicals. However, the marketed tomato contains traces of endosulfán and 4,4'-DDT that are regulated and prohibited in many countries, including Colombia. Tomato quality is stablished according to the Codex Alimentarius recommendations for pesticides, which studies require sensible, selective and probed methods of analysis. Objectives: To report about the estimated average daily intake (EADI) for pesticides residues in the region. In the present work the QuEChERS methodology was modified and validated, based on the EN15662 procedure for the analysis of the organochlorines and organophosphorus pesticides residues in tomato. Methods: The procedure EN15662 was implemented and validated by means of analytical figures of merit from the calibration curve, accuracy analysis and the Youden-Steiner robustness test, for the simultaneous analysis of organochlorines and organophosphorus pesticides using gas chromatography with micro electron capture detector (GC-µECD) in commercialized tomato samples from an organic store Fruver (marketing of vegetables, fresh fruit and vegetables) and 14 grocery stores, for a total of 16 sample points in Armenia. The EADI was estimated for pesticides residues found. Results: A total of 26 residues of pesticides, 20 organochlorines and 6 organophosphorus were analyzed. In mean level of concentration of the calibration curves, recovery was in the range from 82% ± 5 to 136% ± 15 to 17 organochlorines, and in the range from 64% ± 9 to 96% ± 15 to 5 organophosphorus. Other pesticide residues were outside this range of recovery. Detection limits between 0,5 and 257 µg/L and quantification limits between 1,4 and 779 µg/L for aldrin and diazinon, respectively. Conclusions: The methodology used in our studies proves its robustness for the analysis of pesticides. 4,4'-DDT, endosulfán y metoxicloro were found in the majority of samples analyzed, although they are prohibited in Colombia.

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Robustness evaluation of the chromatographic method for the quantitation of lumefantrine using Youden's test

Cited by 42 publications

References 9 publications

Stability Study of Fluconazole Applying Validated Bioassay and Stability-Indicating LC Methods

Stability Study of Fluconazole Applying Validated Bioassay and Stability-Indicating LC Methods

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma

RESIDUOS DE PLAGUICIDAS EN TOMATE (Solanum lycopersicum) COMERCIALIZADO EN ARMENIA, COLOMBIA

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