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1.
J Chromatogr A ; 1730: 465043, 2024 Jun 03.
Artigo em Inglês | MEDLINE | ID: mdl-38908066

RESUMO

In the past few decades, the employment of green analytical approaches in chromatographic method development has attracted the analytical separation community. The greenness of the developed method depends upon the toxicity of solvents and the amount of generated post-analysis waste generated. In this concern, micellar liquid chromatography (MLC) is a simple and rapid technique that generates very low toxic waste compared to traditional chromatographic pesticide detection methods. Here, MLC method has been validated and applied for the determination of monocrotofos (MCF), imidacloprid (ICP), dimethoate (DM) and profenofos (PFF) in spinach and chickpea leaves. The optimized mobile phase was 0.065 M SDS-2 % 1-propanol, 0.01 M NaH2PO4 buffered to pH 7. A C18 column was used for separation with a flow rate of 1 mL/min. The developed method has been validated following the guidelines of SANTE/11,312/2021 and ICH guidelines for; limit of quantification (0.05-0.20 mg/kg), linearity (r2> 0.997-0.999), precision (<6.3 %), accuracy (96.3 %-99.8 %) and robustness (<6) in real samples. ICP and MCF, apart from DM and PFF, were detected in the present work. After detecting insecticides in spinach and chickpea leaves both were washed with different household chemicals i.e. normal, lukewarm, common salt, lemon juice water and commercial ozonizer. Based on five washing techniques with insecticide concentration time intervals reduction rates were calculated for each washing treatment. The results show that lemon juice, common salt water, and ozonizer can be used as washing techniques for the reduction of superficial and systematic residues of ICP and MCF. Common salt and lemon juice water were better for washing over vinegar and potassium permanganate (KMnO4) as they enhance the colour of the green leafy vegetables and are available in every Indian kitchen. They can be easily used by lower socioeconomic classes who cannot afford KMnO4 and vinegar.

2.
Electrophoresis ; 45(3-4): 212-217, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36695087

RESUMO

A procedure to determine albendazole and ivermectin in veterinary formulations, like tablet, bolus, oral suspensions, and injections by micellar liquid chromatography, has been developed. Sample preparation was a batch solid-to-liquid extraction in mobile phase, consisting of a stirring step (15 min), followed by ultrasonication (15 min) and filtration of the obtained supernatant, to reach a target concentration of 2 mg/L for both analytes. Using a mobile phase of 0.15 M sodium dodecyl sulfate-6% 1-pentanol buffered at pH 3 with a 0.01 M phosphate salt, running at 1 mL/min through a C18 column, both drugs were resolved in less than 10 min. Absorbance detection wavelength was 292 nm. Procedure was validated by the guidelines of the International Council on Harmonization in terms of specificity, calibration range (0.025-5 mg/L), trueness (97.8%-102.6%), precision (<2.2%), and system suitability. The method was found easy-to-handle, low cost, safe, green, and with high sample-throughput, thus useful for routine analysis. Therefore, it represents a valuable alternative for quality control of veterinary formulations. It was applied to samples of veterinary formulations purchased from local chemists and veterinarians, and label claims were inside the acceptance criteria (95%-105%).


Assuntos
Albendazol , Ivermectina , Micelas , Cromatografia Líquida/métodos
3.
J Chromatogr A ; 1705: 464206, 2023 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-37481863

RESUMO

Hydroquinone (HQ), resorcinol (RS), m-aminophenol (m-AMP) and p-phenylenediamine (p-PPD) are aromatic compounds which are generally used in hair dyes to provide different colours to hair. In European Union the concentrations of HQ, RS, m-AMP and p-PPD is regulated in hair dyes and other cosmetic products by EU commission regulation EU/2019/831. This legislation is generally exercised because all these compounds are toxic and may cause severe allergies when used regularly. However in India no such regulations exist to monitor these toxic compounds in hair dyes therefore in this study a simple, rapid, economical and ecofriendly micellar liquid chromatographic (MLC) technique has been developed which can monitor all the selected toxic compounds simultaneously. HQ and RS are positional isomers and are difficult to be separated by HPLC whereas with the developed MLC method it was well separated and detected. The developed MLC technique has been applied to detect and quantify selected analytes in oxidative and non-oxidative hair dyes and swab samples from the scalp. The simultaneous separation of selected analytes was performed in mobile phase 0.09 M SDS, 0.01 M NaH2PO4-2% v/v 1-butanol at pH 7 running through C18 column under isocratic mode at 1 mL/min. flow rate. All the analytes were eluted within 6 min. The present method has been validated following the EURCHEM Guideline, 2014 in terms of calibration range (0.08-15 µg/mL), limit of detection (0.01-0.09 µg/mL), limit of quantification (0.08-0.35 µg/mL), accuracy (<5.6%), precision (91-105%) and robustness (<5.8%). The selected compounds in hair dye formulation were found in the range of 0.06-12.2 µg/mL (when diluted 25 times). Hair dyes persistence study was conducted up to 10 days from the day of application on the scalp, suggesting that the dyes were not completely washed off and were retained on the scalp for more than one week. SEM analysis of dyed hair revealed that hair are severely damaged due to use of dyes. The advantage of the developed method is that it could easily be adopted by quality control and cosmetic laboratories for quality control and check for the simultaneous separation of positional isomers together with two other aromatic compounds.


Assuntos
Tinturas para Cabelo , Tinturas para Cabelo/química , Micelas , Cromatografia Líquida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Cabelo
4.
Artigo em Inglês | MEDLINE | ID: mdl-37290211

RESUMO

Combined prescription of the antimicrobial drugs linezolid and meropenem is a common strategy to treat multidrug-resistant nosocomial infections. We propose an innovative method to determine these two drugs in plasma and urine, based on micellar liquid chromatography. Both biological fluids were diluted in mobile phase, filtered and directly injected, without any extraction step. Using a C18 column and a mobile phase of 0.1 M sodium dodecyl sulfate - 10 % methanol, phosphate buffered at pH 3, running under isocratic mode, both antibiotics were eluted without overlapping in<15 min. Detection was by absorbance: 255 nm for linezolid and 310 nm for meropenem. The influence of sodium dodecyl sulfate and methanol concentration on retention factor was established for both drugs using an interpretative approach assisted by chemometrics. The procedure was successfully validated following the guidelines of 2018 Bioanalytical Method Validation Guidance for Industry in terms of: linearity (determination coefficients over 0.99990), calibration range (1 - 50 mg/L), instrumental and method sensitivity, trueness (bias of -10.8 to + 2.4%), precision (relative standard deviation of < 10.2%), dilution integrity, carry-over effect, robustness and stability. It should be emphasized that the method uses low volumes of toxic and volatile solvents and can be achieved in a short period. The procedure was found useful for routine analysis, as it was cost-affordable, more eco-friendly and safer than hydroorganic HPLC, easy-to-handle and highly sample-throughput. Finally, it was applied to incurred samples of patients taking this medication.


Assuntos
Antibacterianos , Infecção Hospitalar , Humanos , Micelas , Meropeném , Linezolida , Infecção Hospitalar/tratamento farmacológico , Dodecilsulfato de Sódio/química , Metanol , Cromatografia Líquida/métodos , Cromatografia Líquida de Alta Pressão
5.
J Chromatogr A ; 1698: 464000, 2023 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-37086546

RESUMO

A method based on micellar liquid chromatography has been developed to determine rosuvastatin, lovastatin and simvastatin in oral solid dosage forms. Samples were solved in mobile phase up to the target concentration, filtered and directly injected. The three statins were resolved in 30 min, using an aqueous solution of 0.10 M sodium dodecyl sulfate - 7.0% 1-butanol, buffered at pH 3 with 0.01 M phosphate salt as mobile phase, running under isocratic mode at 1 mL/min through a C18 column. Detection was at 240 nm. The effect of sodium dodecyl sulfate on elution strength was more important than that of the organic solvent. The procedure was successfully validated by the guidelines of the International Council for Harmonization in terms of: specificity, linearity (r2 > 0.990), calibration range (1.5 - 15 mg/L for rosuvastatin, 0.5-10 mg/L for lovastatin and simvastatin), limit of detection (0.4, 0.2 and 0.15 mg/L for rosuvastatin, lovastatin and simvastatin, respectively), trueness (98.8-101.7%), precision (<2.7%), carry-over effect, robustness, and stability. Values were inside the acceptance criteria of the Methods, Method Verification and Validation, Food and Drug Administration-Office of Regulatory Affairs, thus ensuring the reliability of the results. The main feature was the low proportion of organic solvent used, thus making the procedure sustainable and green. Besides, it was easy-to-conduct and with high sample-throughput, and then useful for routine analysis in pharmaceutical quality control. Finally, it was applied to commercial pharmaceutical preparations.


Assuntos
Inibidores de Hidroximetilglutaril-CoA Redutases , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida/métodos , Lovastatina/análise , Micelas , Reprodutibilidade dos Testes , Rosuvastatina Cálcica , Sinvastatina/análise , Dodecilsulfato de Sódio , Administração Oral
6.
Environ Pollut ; 296: 118719, 2022 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-34952183

RESUMO

Amoxicillin (AMO) and amikacin (AMK) are broad-spectrum antibiotics that are most preferably given post-delivery (normal and cesarian) in the maternity hospitals located in Sagar city (Madhya Pradesh), India. Both the antibiotics make their way through sewage/drainage systems into the environment in the form of metabolized and unmetabolized compounds. Growing concern about the contamination of wastewater by antibiotics requires fast, sensitive and eco-friendly techniques. Therefore a simple, rapid and environmental friendly chromatographic method has been developed for simultaneous determination of AMO and AMK in maternity hospital wastewater samples. A micellar liquid chromatographic (MLC) method was developed with a C18 column (250 mm × 4.6 mm), sodium dodecyl sulphate (SDS; 0.15 M), 1-butanol (7%) as a modifier, pH 5 and photo diode detector (PDA) at 270 nm and 256 nm for AMO and AMK respectively. The method was fast with analysis time below 9 min. In the present MLC method, linearities (r > 0.998), limits of quantification in the range of 0.02-0.04 µg/mL, repeatabilities, and intermediate precision below 4.9% were adequate for the quantification of AMO and AMK. The proposed method can be utilized to detect and quantify both the antibiotics in various samples by hospitals, pharmaceutical companies, pollution control board, municipal corporations, etc.


Assuntos
Amicacina , Amoxicilina , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Feminino , Maternidades , Humanos , Gravidez , Reprodutibilidade dos Testes , Águas Residuárias
7.
Antibiotics (Basel) ; 8(4)2019 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-31731615

RESUMO

A method based on micellar liquid chromatography was developed to determine oxolinic acid, ciprofloxacin, enrofloxacin, and sarafloxacin in eggs and egg products. The antimicrobial drugs were obtained in a micellar solution which was directly injected. The analytes were resolved using a C18 column and a mobile phase of 0.05 M sodium dodecyl sulfate-7.5% 1-propanol-0.5% triethylamine, buffered at pH 3 with phosphate salt, running under the isocratic mode. The signal was monitored by fluorescence. Validation was successfully performed according to the EU Commission Decision 2002/657/EC in terms of specificity, calibration range (LOQ to 1 mg/kg), linearity (R2 > 0.9991), limit of detection and decision limit (0.01-0.05 mg/kg), limit of quantification (0.025-0.150 mg/kg), detection capability (<0.4 times decision limit), trueness (-14.2% to +9.8%), precision (<14.0%), robustness, and stability. The procedure was environmentally friendly, safe, easy-to-conduct, inexpensive, and had a high sample throughput, thus it is useful for routine analysis as a screening method in a laboratory for food residue control.

8.
J Sci Food Agric ; 99(3): 1375-1383, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30120781

RESUMO

BACKGROUND: Micellar liquid chromatography - fluorescence detection was used to determine the antibiotics flumequine, marbofloxacin, difloxacin, and sarafloxacin in porcine, bovine, poultry, ovine, caprine, rabbit, and equine meat, to verify compliance with EU Regulation 37/2010 with regard to the occurrence of veterinary drugs in food. RESULTS: The analytes were isolated from the matrix by ultrasonication-assisted leaching in a micellar solution, and the supernatant was filtered and directly injected. The fluoroquinolones were resolved in < 19 min using a C18 column, with an isocratic mobile phase of 0.05 mol L-1 sodium dodecyl sulfate - 8% 1-butanol - 0.5% triethylamine buffered at pH 3. The limits of quantification (0.01-0.05 mg kg-1 ) were below the maximum residue limits (0.15-0.4 mg kg-1 ). The method was validated by EU Commission Decision 2002/657/EC guidelines. CONCLUSION: The method shows practical advantages such as simplicity, low cost, eco-friendliness, safety, and applicability for routine analysis, and is useful for surveillance programs. © 2018 Society of Chemical Industry.


Assuntos
Antibacterianos/análise , Cromatografia Líquida/métodos , Resíduos de Drogas/análise , Carne/análise , Animais , Bovinos , Ciprofloxacina/análogos & derivados , Ciprofloxacina/análise , Fluoroquinolonas/análise , Contaminação de Alimentos/análise , Cabras , Cavalos , Aves Domésticas , Coelhos , Ovinos , Suínos
9.
Antibiotics (Basel) ; 7(4)2018 Dec 11.
Artigo em Inglês | MEDLINE | ID: mdl-30545003

RESUMO

Isoniazid is a drug that is widely used against tuberculosis. However, it shows high interpatient variability in metabolism kinetics and clinical effect, which complicates the prescription of the medication and jeopardizes the success of the therapy. Therefore, in a specific patient, the pharmacokinetics of the drug must be elucidated to decide the proper dosage and intake frequency to make the drug suitable for therapeutic drug monitoring. This can be performed by the quantification of the drug in urine as this process is non-invasive and allows the effects of long-time exposure to be inferred. The paper describes the development of a micellar liquid chromatographic method to quantify isoniazid in urine samples. Extraction steps were avoided, making the procedure easy to handle and reducing the waste of toxic organic solvents. Isoniazid was eluted in less than 5 min without interference from other compounds of the urine using a mobile phase containing 0.15 SDS⁻12.5% 1-propanol (v/v)⁻Na2HPO4 0.01 M buffered at pH 7, running at 1 mL/min under isocratic mode through a C18 column with the detection wavelength at 265 nm. The method was validated by following the requirements of the Guidelines on Bioanalytical Method Validation issued by the European Medicines Agency (EMA) in terms of selectivity, calibration curve (r² = 0.9998 in the calibration range (0.03⁻10.0 µg/mL), limit of detection and quantification (10 and 30 ng/mL respectively), precision (<16.0%), accuracy (-0.9 to +8.5%), carry-over, matrix effect, and robustness. The developed method was applied to quantify isoniazid in urine samples of patients of an Indian hospital with good results. The method was found to be useful for routine analysis to check the amount of isoniazid in these patients and could be used in its therapeutic monitoring.

10.
Electrophoresis ; 38(16): 2011-2017, 2017 08.
Artigo em Inglês | MEDLINE | ID: mdl-28597925

RESUMO

The suitability of an analytical method to determine oxolinic acid, danofloxacin, ciprofloxacin and enrofloxacin in edible tissues, based on micellar liquid chromatography coupled with fluorescence detection, to be applied in chicken, turkey, duck, lamb, goat, rabbit and horse muscle, is described. The method was fully matrix-matched in-lab revalidated, for each antimicrobial drug and meat, following the guidelines of the EU Commission Decision 2002/657/EC. The permitted limits were the maximum residue limits stated by the EU Commission Regulation 37/2010. The results obtained for the studied validation parameters were in agreement with the guidelines: selectivity (the antibiotics were resolved), linearity (r2  > 0.995), limit of detection (0.004-0.02 mg/kg), limits of quantification (0.01-0.05 mg/kg), calibration range (up to 0.5 mg/kg), recovery (89.5-105.0%), precision (<8.3%), decision limit, detection capability, ruggedness, stability and application to incurred samples. The method was found to be able to provide reliable concentrations with low uncertainty within a large interval, including the maximum residue limits, and then was useful to find out prohibited contaminated samples. The method did not require to be adapted for these matrices, and then it maintained its interesting advantages: short-time, eco-friendly, safe, inexpensive, easy-to-conduct, minimal manipulation and useful for routine analysis.


Assuntos
Antibacterianos/análise , Ciprofloxacina/análise , Fluoroquinolonas/análise , Carne/análise , Ácido Oxolínico/análise , Animais , Galinhas , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Patos , Enrofloxacina , Fluorescência , Cavalos , Humanos , Limite de Detecção , Micelas , Coelhos , Sensibilidade e Especificidade , Ovinos , Perus
11.
Food Chem ; 221: 1277-1284, 2017 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-27979089

RESUMO

A method was developed for the determination of oxolinic acid, danofloxacin, ciprofloxacin and enrofloxacin by micellar liquid chromatography - fluorescence detection in commercial porcine and bovine meat. The samples were ultrasonicated in a micellar solution, free of organic solvent, to extract the analytes, and the supernatant was directly injected. The quinolones were resolved in <22min using a mobile phase of 0.05M SDS - 7.5% 1-propanol - 0.5% triethylamine buffered at pH 3, running through a C18 column at 1mL/min using isocratic mode. The method was validated by the in terms of: selectivity, calibration range (0.01-0.05 to 0.5mg/kg), linearity (r2>0.9998), trueness (89.3-105.1%), precision (<8.3%), decision limit (<12% over the maximum residue limit), detection capability (<21% over the maximum residue limit), ruggedness (<5.6%) and stability. The procedure was rapid, eco-friendly, safe and easy-to-handle.


Assuntos
Anti-Infecciosos/análise , Cromatografia Líquida/métodos , Ciprofloxacina/análise , Resíduos de Drogas/análise , Fluoroquinolonas/análise , Carne/análise , Ácido Oxolínico/análise , Animais , Bovinos , Cromatografia Líquida/instrumentação , Enrofloxacina , Fluorescência , Contaminação de Alimentos/análise , Micelas , Suínos
12.
Bioanalysis ; 8(12): 1225-35, 2016 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-27241819

RESUMO

BACKGROUND: Micellar LC was first proposed as a 'green' mode using mobile phases of water and surfactant. However, in most procedures a small amount of organic solvent is required to decrease the retention to convenient values. Results & methodology: Mixed micellar mobile phases prepared with both cationic (sodium dodecyl sulphate) and nonionic surfactant (Brij-35) modulate the retention of high to moderately polar basic drugs to practical times, eliminating the need of organic solvent. While the mobile phase is continuously recycled through the system, the stationary phase performance is maintained after repetitive injection of the samples. DISCUSSION & CONCLUSION: Through an extensive validation, the approach is shown to be appropriate to determine these drugs in urine samples without previous pretreatment.


Assuntos
Cromatografia Líquida/métodos , Micelas , Preparações Farmacêuticas/urina , Polietilenoglicóis/química , Dodecilsulfato de Sódio/química , Tensoativos/química , Análise de Injeção de Fluxo/métodos , Humanos , Limite de Detecção , Água/química
13.
J Environ Sci (China) ; 42: 284-292, 2016 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-27090721

RESUMO

A method based on micellar liquid chromatography has been developed to simultaneously monitor four pesticides largely post-harvest applied to citrus: thiabendazole, pyrimethanil, o-phenylphenol and imazalil. Water samples were filtered and directly injected without other treatment, thus avoiding extraction steps. The composition of the mobile phase was optimized using a chemometrical approach to achieve and excellent resolution to 0.07 mol/L SDS/5%, V/V 1-pentanol buffered at pH3. Mobile phase run through a C18 column at 1 mL/min at room temperature. The detection was performing by UV-Visible absorbance using a wavelength program: 0-10 min, 305 nm (for thiabendazole); 10-12; 265 nm (for pyrimethanil) and 12-18, 220 nm (o-phenylphenol and imazalil). The developed method was validated following the guidelines of the US Environmental Protection Agency in terms of: quantitation range, (0.5-4 to 15 µg/mL), linearity (r(2)>0.9995), sensitivity (LOD, 0.18-1.4 µg/mL), precision (<9.2%), trueness (93.9%-103.7%), and ruggedness (<9.9%). It was found that the fungicides remain up to eight days in surface water at outdoor conditions. The method was used to screen the presence of the analytes in several waste water samples, and was proved to be useful in routine analysis.


Assuntos
Monitoramento Ambiental/métodos , Fungicidas Industriais/análise , Águas Residuárias/química , Poluentes Químicos da Água/análise , Agricultura , Cromatografia Líquida , Citrus , Micelas
14.
Analyst ; 140(5): 1739-46, 2015 Mar 07.
Artigo em Inglês | MEDLINE | ID: mdl-25604004

RESUMO

A micellar liquid chromatographic method has been developed for the simultaneous quantification of the pesticides thiabendazole and chlorpyrifos, as well as an alkylphenol, which is included in pesticide formulations, i.e., 4-tert-octylphenol, in water. A sample was filtered and directly injected, avoiding large extraction steps using toxic solvents, thus expediting the experimental procedure. The contaminants were eluted without interferences in <17 min, using a mobile phase of 0.15 M sodium dodecyl sulfate ­ 6% 1-pentanol buffered at pH 3, running through a C18 column at 1 mL min(-1) under the isocratic mode. This optimal mobile phase was selected using a statistical approach, which considers the retention factor, efficiency and peak shape of the analytes measured in only a few mobile phases. The detection was carried out by measuring absorbance at 220 nm. The method was successfully validated in terms of specificity, calibration range (0.5-10 mg L(-1)), linearity (r(2) > 0.994), limit of detection and quantification (0.2-0.3; and 0.5-0.8 mg L(-1), respectively), intra- and interday accuracy (95.2-102.9%), precision (<8.3%), and ruggedness (<9.3%). The stability in storage conditions (at least 14 days) was studied. The method was safe, inexpensive, produced little pollutant and has a short analysis time, thus it is useful for the routine analysis of samples. Finally, the method was applied to analyse wastewater from the fruit-processing industry, wastewater treatment plants, and in sewage water belonging to the Castelló area (Spain). The results were similar to those obtained by an already reliable method.


Assuntos
Clorpirifos/análise , Cromatografia Líquida/instrumentação , Cromatografia Líquida/métodos , Fenóis/análise , Tiabendazol/análise , Águas Residuárias/análise , Micelas , Esgotos/análise
15.
J Lab Autom ; 20(3): 259-64, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25304875

RESUMO

Classical microbiological methods currently have unacceptably long cycle times. Rapid microbiological methods have been available on the market for decades and have been applied by the clinical and food industries. However, their implementation in the pharmaceutical industry has been hampered by stringent regulations on validation and comparison with classical methods. To encourage the implementation of these methodologies, they must be validated to assess that the results are straightforward. A comparison with traditional methods should be also performed. In this review, information about the validation of rapid microbiological methods reported in the literature is provided as well as an explanation of the difficulty of validation of these methods. A comparison with traditional methods is also discussed. This information is useful for industries and laboratories that can potentially implement these methods.


Assuntos
Biotecnologia/métodos , Técnicas Microbiológicas/métodos , Animais , Humanos , Guias de Prática Clínica como Assunto , Reprodutibilidade dos Testes , Estudos de Validação como Assunto
16.
Mini Rev Med Chem ; 14(10): 831-6, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25342195

RESUMO

In the last ten years, a high amount of genetic assays has been developed for molecular biopathology and genetic laboratories of the hospitals, mainly developed and provided by external companies. In some cases, the specialized staff members of the hospitals (doctors, biopathologists, geneticists or pharmacists) develop their own methods. The validation of these methods is required before their use in clinical testing, in order to assess its reliability. Analytical methods are validated under the requirements of International Guidelines, but validation procedures for clinical genetic tests are under study and need clarifications. In this manuscript, the main information related to the field of genetic validation is revised, including statistics, explaining the difficulty of validation for some of the developed genetic tests. The provided information is in agreement with all the International Guides. The information could be useful by the workers daily performing this kind of analysis.


Assuntos
Testes Genéticos/normas , Calibragem , Testes Genéticos/métodos , Humanos , Padrões de Referência , Reprodutibilidade dos Testes , Estudos de Validação como Assunto
17.
Anal Sci ; 30(9): 925-30, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25213822

RESUMO

This paper describes a micellar liquid chromatographic method used to analyze tamoxifen (TAMO) in pharmaceutical formulations, while focusing in its interesting features. Solid samples were solved in a micellar solution, irradiated at 254 nm, filtered and injected. Extraction steps were avoided and thus expediting the procedure. Tamoxifen was resolved in <5 min, using a mobile phase containing 0.15 M sodium dodecyl sulfate-7% pentanol at pH 3, running at 1.5 mL/min under an isocratic mode at 40°C through a C18 column. Detection was achieved by fluorescence by excitation at 260 nm and emission at 380 nm. The validation was performed following the requirements of the International Conference on Harmonization (ICH) Tripartite Guidelines in terms of: specificity, sensitivity, calibration range (0.2 - 20 mg/L), accuracy (98.8 - 101.7%), precision (<1.5%) and robustness (<6.2%). The method was applied to quantify TAMO in TAMO citrate tablets supplied in Spain, and was found appropriate for the quality control of TAMO formulations.


Assuntos
Cromatografia Líquida/métodos , Preparações Farmacêuticas/química , Moduladores Seletivos de Receptor Estrogênico/análise , Tamoxifeno/análise , Cromatografia Líquida/instrumentação , Limite de Detecção , Preparações Farmacêuticas/normas , Comprimidos
18.
J Sep Sci ; 37(20): 2825-32, 2014 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-25103282

RESUMO

Danuravir, ritonavir, emtricitabine, and tenofovir are together prescribed against AIDS as a highly active antiretroviral therapy regimen. Micellar liquid chromatography has been applied to determine these four antiretroviral drugs in plasma. The sample preparation is shortened to the dilution of the sample in a micellar solution, filtration, and injection. Clean-up steps are avoided, due to the solubilization of plasma matrix in micellar media. The drugs were analyzed in <20 min using a mobile phase of 0.06 M sodium dodecyl sulfate/2.5% 1-pentanol (pH 7) running under isocratic mode through a C18 column at 1 mL/min at room temperature. Absorbance wavelength detection was set at 214 nm. The method was successfully validated following the ICH Harmonized Tripartite Guideline in terms of selectivity, limit of detection (0.080-0.110 µg/mL), limit of quantification (0.240-0.270 µg/mL), linearity between 0.25 and 25 µg/mL (r(2) > 0.995), accuracy (89.3-103.2%), precision (<8.2%) and robustness (<7.5%). Real plasma sample from patients taking this therapy were analyzed. This is the first paper showing the simultaneous detection of this four drugs. Therefore, the methodology was proven useful for the routine analysis of these samples in a hospital laboratory for clinical purposes.


Assuntos
Fármacos Anti-HIV/sangue , Cromatografia Líquida/métodos , Micelas , Adenina/análogos & derivados , Adenina/sangue , Calibragem , Darunavir , Desoxicitidina/análogos & derivados , Desoxicitidina/sangue , Emtricitabina , Humanos , Organofosfonatos/sangue , Ritonavir/sangue , Dodecilsulfato de Sódio/química , Sulfonamidas/sangue , Tenofovir
19.
J Pharm Biomed Anal ; 98: 351-5, 2014 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-24996008

RESUMO

An analytical methodology based on micellar liquid chromatography has been developed to quantify abacavir, lamivudine and raltegravir in plasma. These three antiretroviral drugs are prescribed as a set in highly active antiretroviral therapy to acquired immunodeficiency syndrome patients. The experimental procedure consists in the dilution of the sample in micellar media, followed by filtration and, without cleanup step. The analytes were resolved in less than 30min using a mobile phase of 0.05M sodium dodecyl sulphate at pH 7, running at 1mLmin(-1) under isocratic mode at room temperature through a C18 column (125×4.6mm, 5µm particle size). The UV detection wavelength was set at 260nm. The method was successfully validated following the requirements of ICH guidelines in terms of: linear range (0.25-2.5µgmL(-1)), linearity (r(2)>0.990), intra- and interday precision (<6.8%) and accuracy (92.3-104.2%) and robustness (<7.1%). To the extent of our knowledge, this is the first published method to quantify these three drugs in plasma. Several blood samples from AIDS patients taking this HAART set provided by a local hospital were analyzed with satisfactory results.


Assuntos
Didesoxinucleosídeos/sangue , Didesoxinucleosídeos/química , Lamivudina/sangue , Lamivudina/química , Plasma/química , Pirrolidinonas/sangue , Pirrolidinonas/química , Antirretrovirais/sangue , Antirretrovirais/química , Terapia Antirretroviral de Alta Atividade/métodos , Cromatografia Líquida/métodos , Micelas , Raltegravir Potássico , Dodecilsulfato de Sódio/química
20.
Artigo em Inglês | MEDLINE | ID: mdl-25023211

RESUMO

Citalopram, paroxetine and fluoxetine are selective serotonin reuptake inhibitor (SSRIs) currently used in the treatment of psychiatric disorders. We present an analytical method using micellar liquid chromatography to quantify these three drugs in pharmaceutical formulations, plasma and urine. The resolution was performed using a mobile phase of 0.075 M SDS - 6% (v/v) butanol buffered at pH 7 running through a C18 column under isocratic mode at 1 mL/min at 25°C. The analytes were eluted in less than 20 min. The fluorescence detection was programmed at the maximum excitation (236, 295 and 230 nm) and emission (310, 350 and 305 nm) wavelengths for citalopram, paroxetine and fluoxetine, respectively. The experimental procedure was expedited to 1/5 dilution of the sample in the micellar mobile phase and filtration, thus avoiding clean-up and extraction steps. An aliquot of 20 µL was injected after 80 min of preparation, to obtain maximum sensitivity. The method was validated according to the guidelines of the Food and Drug Administration (FDA) in terms of calibration range (20-500 ng/mL; r(2)>0.999), sensitivity, accuracy (91.3-103.2%), precision (<9.3%), and robustness (<6.1%). The suitability of the method was successfully evaluated by analyzing plasma and urine samples from patients treated with SSRIs and checking the content of the active principle in tablets. Thus, the method can be applied to pharmacokinetics studies and in forensic cases, as well as in quality control of commercial pharmaceutical formulations.


Assuntos
Cromatografia Líquida/métodos , Inibidores Seletivos de Recaptação de Serotonina/sangue , Inibidores Seletivos de Recaptação de Serotonina/urina , Espectrometria de Fluorescência/métodos , Antidepressivos/sangue , Antidepressivos/urina , Humanos , Análise dos Mínimos Quadrados , Micelas , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Estereoisomerismo
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