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Разработка и валидация метода количественного определения декскетопрофена трометамола в плазме крови человека А. П. Лакеев

By: Лакеев, Александр ПавловичMaterial type: ArticleArticleContent type: Текст Media type: электронный Other title: Development and validation method for quantitative determination of the dexketoprofen trometamol in human plasma [Parallel title]Subject(s): декскетопрофен | плазма крови человека | нестероидные противовоспалительные препараты | экспериментальные исследованияGenre/Form: статьи в сборниках Online resources: Click here to access online In: Перспективы развития фундаментальных наук. Т. 2 : сборник научных трудов XVII Международной конференции студентов, аспирантов и молодых ученых, Россия, Томск, 21-24 апреля 2020 г Т. 2 : Химия. С. 104-106Abstract: Dexketoprofen (DKP) belongs to the group of nonsteroidal anti-inflammatory drugs exhibiting expressed biological properties. Typically, the concentration of the drug in human plasma is very low, generally in the ng/ml range. Therefore, the aim was to develop and validate a rapid, accurate, precise, reproducible and highly sensitive HPLC-MS/MS method for the quantitative analysis of DKP in the specified samples. DKP was separated on a Phenomenex Luna С18 column (3 fim, 50^2 mm) at 40°C and analysed in positive-ion electrospray ionization mode. The mobile phase consisted of acetonitrile:0.1% formic acid (60:40, v/v) under isocratic conditions at a flow rate of 0.30 ml/min. The samples were extracted using ethyl acetate with the addition of 0.6 M sulfuric acid and ibuprofen (IBP) as internal standard. Subsequently, the upper organic phase was isolated and 2 il samples were injected onto column for analysis. DKP and IBP eluted at 1.62 ± 0.02 и 2.43 ± 0.03 min, respectively. The total analysis time was 3.5 min. DKP and IBP responses were optimised at the transitions (m/z) 255.2 ^ 105.2 and 206.2 ^ 161.2, respectively. Calibration curves were linear over the range 10-8500 ng/ml with correlation coefficients > 0.999. The method was successfully applied to determine the bioavailability of DKP after a single dose on an empty stomach by volunteers.
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Dexketoprofen (DKP) belongs to the group of nonsteroidal anti-inflammatory drugs exhibiting expressed biological properties. Typically, the concentration of the drug in human plasma is very low, generally in the ng/ml range. Therefore, the aim was to develop and validate a rapid, accurate, precise, reproducible and highly sensitive HPLC-MS/MS method for the quantitative analysis of DKP in the specified samples. DKP was separated on a Phenomenex Luna С18 column (3 fim, 50^2 mm) at 40°C and analysed in positive-ion electrospray ionization mode. The mobile phase consisted of acetonitrile:0.1% formic acid (60:40, v/v) under isocratic conditions at a flow rate of 0.30 ml/min. The samples were extracted using ethyl acetate with the addition of 0.6 M sulfuric acid and ibuprofen (IBP) as internal standard. Subsequently, the upper organic phase was isolated and 2 il samples were injected onto column for analysis. DKP and IBP eluted at 1.62 ± 0.02 и 2.43 ± 0.03 min, respectively. The total analysis time was 3.5 min. DKP and IBP responses were optimised at the transitions (m/z) 255.2 ^ 105.2 and 206.2 ^ 161.2, respectively. Calibration curves were linear over the range 10-8500 ng/ml with correlation coefficients > 0.999. The method was successfully applied to determine the bioavailability of DKP after a single dose on an empty stomach by volunteers.

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