RESUMO
Resumen Se identificaron los componentes aromáticos activos provenientes de muestras comerciales del aceite de sacha inchi, obtenidos de cultivos de Santa Rosa de Osos (Antioquia, Colombia), mediante la técnica de microextracción en fase sólida acoplada a cromatografía de gases, espectrometría de masas y olfatometría (HS-SPME-GC-MS-O). En la optimización de la técnica de extracción se definieron las siguientes condiciones: fibra de SPME de divinilbenceno/ carboxen/polidimetilsiloxano (DVB/CAR/PDMS), temperatura de extracción de 50 °C y tiempo de exposición de 40 min. Bajo estas condiciones, se encontraron un total de 20 compuestos aromáticos activos, donde se destacan el E-2-octenal, E-heptanal, (E,E)-3,5-octadien-2-ona, ácido hexanóico y (E,E)-2,4-heptadienal como los componentes con mayor aporte a la formación del aroma del aceite de sacha inchi.
Abstract The active aromatic components from commercial samples of sacha inchi oil obtained from Santa Rosa de Osos (Antioquia, Colombia) crops were identified by solid phase microextraction technique coupled to gas chromatography, mass spectrometry, and olfactometry (HS -SPME-GC-MS-O). In the optimization of the extraction technique, the following conditions were defined: SPME fiber of divinylbenzene/carboxen/ polydimethylsiloxane (DVB/CAR/PDMS), extraction temperature 50 °C, and exposure time 40 min. Under these conditions, a total of 20 active aromatic compounds were found, which include E-2-octenal, E-heptanal, (E,E)-3,5-octadien-2-one, hexanoic acid and (E,E)-2,4-heptadienal as the components with the greatest contribution to the aroma formation of sacha inchi oil.
Resumo Os componentes de aroma ativos de amostras comerciais de óleo de sacha inchi obtidos de Santa Rosa de Osos (Antioquia, Colômbia) foram separados pela técnica de microextração em fase sólida acoplada a cromatografia gasosa, espectrometria de massas e olfatometria para a identificação (HS-SPME-GC-MS-O). Na otimização da técnica de extração, foram definidas as seguintes condições: fibra de SPME de divinilbenzeno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS), temperatura de extração 50 °C e tempo de exposição de 40 min. Nestas condições, foi encontrado um total de 20 compostos de aroma ativos no óleo, que incluem E-2-octenal, E-heptanal, (E,E)-3,5-octadien-2-ona, ácido hexanoico e (E,E)-2,4 heptadienal como os componentes com maior contribuição para a formação do aroma.
RESUMO
One of the most important aspects regarding the therapeutic efficacy of antimalarials is its quantification in biologic fluids. The detection and measurement of antimalarial drug levels is important for demonstrating (1) adequate absorption of the drug being given, (2) compliance in taking the full regimen required for treatment and (3) the level of drug in the blood at any time during the test period that parasites reappear. There is a lack of validated methods that simultaneously quantify different antimalarials administered at the same time, such as the use of chloroquine (CQ) and primaquine (PQ) in infections caused by Plasmodium vivax. In this study, a bioanalytical method was validated for the simultaneous quantification of primaquine (PQ), chloroquine (CQ) and desethylchloroquine (DSCQ) in human plasma using liquid-liquid extraction and high performance liquid chromatography with a diode array detector (HPLC-DAD). The PQ was evaluated over a concentration range of 100-3000 nM and the CQ and DSCQ was evaluated over a concentration range of 20-2000 nM. The selectivity of the method was verified by checking for interference by commonly used antimalarials and plasma samples. The accuracy and precision of the method was assessed for drugs spiked into human plasma and recoveries of 83.7%, 92.3%, and 76.5% were obtained for CQ, DSCQ, and PQ, respectively. The applicability of this method was also demonstrated with blood samples from patients with vivax malaria that received combination CQ plus PQ treatment. The simultaneous detection and accurate measurement of CQ, DSCQ, and PQ levels in human plasma provides an important and economical method for validating and monitoring sensitivity/resistance of P. vivax to more common treatment regimen.
Assuntos
Cloroquina/análogos & derivados , Cloroquina/sangue , Cromatografia Líquida de Alta Pressão/métodos , Primaquina/sangue , Calibragem , Humanos , Limite de Detecção , Malária Vivax/tratamento farmacológicoRESUMO
Objective: to validate an analytical method for simultaneous determination and quantification of sulphadoxine and pyrimethamine in human blood dried onto filter paper, whose cost and analysis time can be reduced. Methods: whole blood spotted on filter paper of a healthy volunteer and solutions of sulphadoxine-pyrimethamine standard mixture were used. HPLC separations were carried out on Agilent equipment using a LiChrospher® column C18 with a mobile phase acetonitrile/0.1 M potassium phosphate buffer at pH 3.0 (1:1) for eight minutes under isocratic conditions. A flow rate of 0.7 mL/min, and a 20 mL volume injection were used. External standard method for quantitation of analytes was used. Results: the HPLC method described for the simultaneous determination of sulphadoxine and pyrimethamine in 100 mL of whole blood spotted on filter paper has been found to be linear, precise, accurate and selective. In this method, the sample preparation is simple using liquid-liquid extraction, and HPLC with ultraviolet detection is used. Conclusions: a simple, fast and sensitive method for determination of sulphadoxine and pyrimethamine in human blood dried onto filter paper was validated. This method can be used for the monitoring of both metabolites in pharmacokinetic and clinical studies.
Objetivo: validar un método de análisis para la determinación y cuantificación simultánea de sulfadoxina y pirimetamina en sangre humana secada sobre papel de filtro que sea rápido y barato. Métodos: se usó sangre de un voluntario sano impregnada sobre papel de filtro y soluciones estándar de la mezcla sulfadoxina y pririmetamina. Las separaciones por cromatografía líquida de alta resolución (CLAR) se hicieron en un equipo Agilent sobre una columna C18 LiChrospher® con acetonitrilo/buffer fosfato de potasio 0,1 M a pH 3,0 como fase móvil, usando condiciones isocráticas durante 8 min. Se usó un flujo de 0,7 mL/min y un volumen de inyección de 20 mL. Para la cuantificación de los analitos se utilizó el método del estándar externo. Resultados: el método CLAR descrito para la determinación simultánea de sulfadoxina y pirimetamina en 100 mL de sangre impregnada sobre el papel de filtro mostró linealidad, precisión, exactitud y selectividad. En este método la preparación de la muestra es simple ya que usa extracción líquido-líquido y detección ultravioleta. Conclusión: se obtuvo un método validado que es simple, rápido y sensible para la determinación de sulfadoxina y pirimetamina en sangre humana impregnada sobre papel de filtro, que puede ser usado para el monitoreo de ambos metabolitos en estudios farmacocinéticos y clínicos.