Browsing by Subject "High performance liquid chromatography"
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- PublicationOpen AccessA novel liquid chromatography-fluorescence method for the determination of delafloxacin in human plasma(Wiley, 2022-02-05) Hernandis Belenguer, Verónica; Escudero Pastor, Elisa; Marín Carrillo, Pedro; FarmacologíaDelafloxacin is a novel fluoroquinolone antibiotic that was approved by the European Medicine Agency to treat bacterial infections of the skin and underlying tissues, and community-acquired pneumonia. Despite being in the market since 2019 in the European Union, there is no published liquid chromatography-fluorescence method for delafloxacin quantification in biological samples. A novel, rapid, and sensitive high-performance liquid chromatographic method was developed to determine delafloxacin in human plasma using its native fluorescence. Plasma delafloxacin concentrations were determined by reverse-phase chromatography with fluorescence detection at 405/450 nm of excitation/emission wavelengths. Delafloxacin was separated on a Kromasil C18 column 250 × 4.6 mm id, 5 µm using isocratic elution. The mobile phase was a mixture of 0.05% trifluoroacetic acid/acetonitrile (52/48). Retention times were 5.4 and 11.6 min for delafloxacin and valsartan (internal standard), respectively. Regression calibration curves were linear over the range of 0.1–2.5 µg/mL. The lower limit of detection was 0.05 µg/mL, and the lower limit of quantification was 0.1 µg/mL. Accuracy and precision were always <11%, and the limit of quantification was <16%. Mean recovery was 98.3%. This method can be applied to determine delafloxacin in human plasma and could be useful to perform pharmacokinetic studies.
- PublicationOpen AccessDilute-and-shoot-liquid chromatography-quadrupole time of flight-mass spectrometry for pteridine profiling in human urine and its association with different pathologies(MDPI, 2023-06-01) Giménez Campillo, Claudia; Pastor Belda, Marta; Arroyo Manzanares, Natalia; Campillo Seva, Natalia; Val Oliver, Blanca del; Zarauz García, José; Sáenz, Luis; Viñas López-Pelegrin, Pilar; Química AnalíticaPteridines are a group of compounds synthesised by many living organisms that are involved in the metabolism of many cofactors and vitamins. Their concentration in biological fluids may be altered by various pathologies such as cancer or inflammatory bowel disease, urine being the main route of excretion. In this study, three lumazines and ten pterins were analysed in their native oxidation state using high-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry. Their high concentration in urine samples and their good ionisation behaviour allow the use of the dilute-and-shoot method by simple filtration of the urine prior to chromatographic analysis. The final method offers excellent linearity, sensitivity and precision parameters, and a total of 135 urine samples were analysed from patients with some relevant information such as faecal calprotectin (FCP) levels, common diseases such as diabetes, hypertension and dyslipidaemia and immunological diseases such as inflammatory bowel disease (IBD). The pteridine profile was related to FCP levels without showing any correlation. In addition, pteridine levels were compared between healthy subjects and IBD, diabetic, hypertensive and dyslipidaemic patients, and significant differences were found between the two groups for some of the pteridines.