scholarly journals Razvoj SPE-HPLC-DAD metode za određivanje florfenikola i florfenikol amina u cerebrospinalnoj tekućini svinja

2020 ◽  
Vol 51 (2) ◽  
pp. 129-138
Author(s):  
Ksenija Šandor ◽  
Svjetlana Terzić ◽  
Anja Vujnović ◽  
Eleonora Perak Junaković ◽  
Irena Žarković ◽  
...  
Keyword(s):  
Cerebrospinal Fluid ◽  
High Performance ◽  
Solid Phase ◽  
Biological Fluids ◽  
Experimental Period ◽  
Intramuscular Administration ◽  
Array Detector ◽  
Control Group ◽  
Pharmacokinetic Studies ◽  
Experimental Conditions

A study of florfenicol (FF) and its metabo- lite florfenicol amine (FFA) in pig cerebrospinal fluid was conducted following repeated intramuscular administration of the original (reference) and a generic veterinary medicinal product (VMP) under the same experimental conditions (20 mg FF/kg body weight, 48-hour interval). Both VMPs are solutions for injection containing FF as an active substance in the concentration of 300 mg/mL and have been authorized in Croatia for use in cattle and pigs. In this study, clinically healthy pigs were randomly divided into three groups. The first group was treated with the reference VMP, the second with the generic VMP, while the third served as the control group. Animals were sacrificed at 216, 288 and 384 hours after the first drug administration. Cerebrospinal fluid samples were analysed by the optimized and validated high-performance liquid chromatography-diode array detector method (HPLC-DAD). The solid-phase extraction (SPE) technique was chosen for sample preparation. The HPLC-DAD method provides good linearity over the concentration range of 0.05 to 5.00 μg/mL for FF and FFA. Limits of detection were 0.0023 μg/mL for FF and 0.0100 μg/mL for FFA. Extraction recoveries of FF were from 86.6% to 111.8%, and of FFA from 91.7% to 98.8%. The SPE-HPLC-DAD method has been demonstrated to be a selective, sensitive and suitable analytical method for the determination of FF and FFA in cerebrospinal fluid. The present study was based on a preliminary study that quantified FF in pig plasma at 216 hours after the first application of reference or generic VMP. However, FF and FFA were not detected in any of the cerebrospinal fluid samples during the experimental period. According to the nature of biological fluids, the SPE-HPLC-DAD method can be suitable for further pharmacokinetic studies of FF in pig plasma and serum after intramuscular administration of VMPs.

scholarly journals Metabolic Evaluation of Urine from Patients Diagnosed with High Grade (HG) Bladder Cancer by SPME-LC-MS Method

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2194
Author(s):  
Kamil Łuczykowski ◽  
Natalia Warmuzińska ◽  
Sylwia Operacz ◽  
Iga Stryjak ◽  
Joanna Bogusiewicz ◽  
...  
Keyword(s):  
Thin Film ◽  
Bladder Cancer ◽  
High Performance ◽  
Biomarker Discovery ◽  
Solid Phase ◽  
Biological Fluids ◽  
Reversed Phase ◽  
Control Group ◽  
Metabolic Evaluation ◽  
Metabolomic Profiling

Bladder cancer (BC) is a common malignancy of the urinary system and a leading cause of death worldwide. In this work, untargeted metabolomic profiling of biological fluids is presented as a non-invasive tool for bladder cancer biomarker discovery as a first step towards developing superior methods for detection, treatment, and prevention well as to further our current understanding of this disease. In this study, urine samples from 24 healthy volunteers and 24 BC patients were subjected to metabolomic profiling using high throughput solid-phase microextraction (SPME) in thin-film format and reversed-phase high-performance liquid chromatography coupled with a Q Exactive Focus Orbitrap mass spectrometer. The chemometric analysis enabled the selection of metabolites contributing to the observed separation of BC patients from the control group. Relevant differences were demonstrated for phenylalanine metabolism compounds, i.e., benzoic acid, hippuric acid, and 4-hydroxycinnamic acid. Furthermore, compounds involved in the metabolism of histidine, beta-alanine, and glycerophospholipids were also identified. Thin-film SPME can be efficiently used as an alternative approach to other traditional urine sample preparation methods, demonstrating the SPME technique as a simple and efficient tool for urinary metabolomics research. Moreover, this study’s results may support a better understanding of bladder cancer development and progression mechanisms.

Solid-phase structures of cerebrospinal fluid in diagnosis of early asymptomatic neurosyphilis

2018 ◽  
pp. 56-61
Author(s):  
С.Н. Шатохина ◽  
Н.А. Кузнецова ◽  
В.Н. Шабалин
Keyword(s):  
Cerebrospinal Fluid ◽  
Visual Analysis ◽  
Solid Phase ◽  
Biological Fluids ◽  
Laboratory Methods ◽  
Phase Structures ◽  
Morphological Picture ◽  
Diagnostic Technology

Цель проведённого исследования состояла в оценке эффективности визуального анализа твёрдофазных структур спинномозговой жидкости для диагностики ранних форм нейросифилиса. Методы. Использован метод краевой дегидратации биологических жидкостей, входящий в состав авторской диагностической технологии «Литос-система». Диагностика раннего асимптомного нейросифилиса заключается в выявлении деструктивных образований в форме овалов в морфологической картине твёрдой фазы спинномозговой жидкости. Результаты. Проведён сравнительный анализ результатов исследования спинномозговой жидкости у 19 больных с подтверждённым диагнозом «ранний асимптомный нейросифилис», полученных традиционными лабораторными методами и методом краевой дегидратации. Выявлено, что локализация овалов внутри сферолитов указывает на длительность заболевания нейросифилисом менее трёх лет, а вне сферолитов - от трех до пяти лет. Заключение. Метод краевой дегидратации позволяет диагностировать ранний асимптомный нейросифилис по наличию деструктивных образований в форме овалов в морфологической картине твёрдой фазы спинномозговой жидкости. The aim of this study was to evaluate effectiveness of visual analysis of solid-phase structures in cerebrospinal fluid to diagnose early forms of neurosyphilis. Methods. We used a method of marginal dehydration of biological fluids as a part of the author’s diagnostic technology, Litos-System. Early asymptomatic neurosyphilis is diagnosed based on detection of destructive, oval-shaped formations in the morphological picture of cerebrospinal fluid solid phase. Results. Data from analyses of cerebrospinal fluid performed with traditional laboratory methods and the method of marginal dehydration were compared for 19 patients with documented diagnosis of early asymptomatic neurosyphilis. A localization of ovals within spherulites indicated a less than a three-year duration of neurosyphilis while a localization outside spherulites indicated a duration of three to five years. Conclusion. The method of marginal dehydration allows detecting early asymptomatic neurosyphilis based on the presence of destructive, oval-shaped formations in the morphological picture of cerebrospinal fluid solid phase.

scholarly journals Characterization of Volatile and Flavonoid Composition of Different Cuts of Dried Onion (Allium cepa L.) by HS-SPME-GC-MS, HS-SPME-GC×GC-TOF and HPLC-DAD

Molecules ◽  
2020 ◽  
Vol 25 (2) ◽  
pp. 408 ◽  
Author(s):  
Lorenzo Cecchi ◽  
Francesca Ieri ◽  
Pamela Vignolini ◽  
Nadia Mulinacci ◽  
Annalisa Romani
Keyword(s):  
Gas Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Array Detector ◽  
Volatile Fraction ◽  
Solid Phase Micro Extraction ◽  
Food Ingredient ◽  
Head Space ◽  
Dipropyl Disulfide ◽  
Allium Cepa L

Onion is widely used worldwide in various forms for both food and medicinal applications, thanks to its high content of phytonutrients, such as flavonoids and volatile sulfur compounds. Fresh onion is very perishable and drying is widely applied for extending shelf-life, thus obtaining a very easy-to-use functional food ingredient. The flavonoid and volatile fractions of different onion cuts (flakes, rings) prepared through different drying cycles in a static oven, were characterized by high-performance liquid chromatography with a diode-array detector HPLC-DAD, Head Space-Solid Phase Micro Extraction followed by Gas Chromatography coupled with Mass Spectrometry (HS-SPME-GC-MS) and Head-Space Solid Phase Micro Extraction followed by comprehensive two-dimensional Gas-Chromatography (HS-SPME-GC×GC-TOF). Onion flakes showed a significantly higher flavonoid content (3.56 mg g−1) than onion rings (2.04 mg g−1). Onion flakes showed greater amount of volatile organic compounds (VOCs) (127.26 mg g−1) than onion rings (42.79 mg g−1), with different relative amounts of di- and trisulfides—disulfides largely predominate the volatile fraction (amounts over 60% on the total volatile content), followed by trisulfides and dipropyl disulfide and dipropyl trisulfide were the most abundant VOCs. HS-SPME-GC×GC-TOF allowed for the detection of the presence of allylthiol, diethanol sulfide, 4,6-diethyl1,2,3,5-tetrathiolane, not detected by HS-SPME-GC-MS, and provided a fast and direct visualization and comparison of different samples. These results highlight different nutraceutical properties of dried onion samples processed otherwise, only differing in shape and size, thus pointing out potentially different uses as functional ingredients.

Determination of Ibuprofen and Phenylephrine in Tablets by High-Performance Thin Layer Chromatography and in Plasma by High-Performance Liquid Chromatography with Diode Array Detection

2019 ◽  
Vol 57 (7) ◽  
pp. 592-599
Author(s):  
Marwa A A Ragab ◽  
Mohamed H Abdel-Hay ◽  
Hytham M Ahmed ◽  
Sara M Mohyeldin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Biological Fluids ◽  
Array Detector ◽  
Diode Array ◽  
Simultaneous Extraction ◽  
Layer Chromatography

Abstract Two chromatographic methods (high performance thin layer chromatography (HPTLC) and high performance liquid chromatography–diode array detector (HPLC-DAD)), were addressed for the analysis of a mixture consisted of phenylephrine hydrochloride and ibuprofen in two forms bulk and their combined dosage form. This binary mixture is considered to be a challenging one as the two drugs differ greatly in their chemical and physical properties. Not only this affects their simultaneous analysis, but also hinders their simultaneous extraction from biological fluids as plasma. That is the reason the literature lacks any report for the simultaneous extraction and analysis of these drugs from biological fluids. The concentration ranges of both drugs were 0.1–2.5 μg/spot and 0.1–100 μg/mL by HPTLC and HPLC, respectively. Not only was the HPLC-DAD method applied to the investigated drugs determination in pharmaceutical preparations, but also in spiked human plasma. Extensive study was conducted to optimize their simultaneous extraction from plasma as it was a crucial step for the in vivo analysis. The results obtained by proposed methods and a reference one were statistically comparable by analysis of variance test. No significant difference was recorded between the mean percent levels determined by the proposed methods and the reference one.

scholarly journals Mediterranean Propolis from the Adriatic Sea Islands as a Source of Natural Antioxidants: Comprehensive Chemical Biodiversity Determined by GC-MS, FTIR-ATR, UHPLC-DAD-QqTOF-MS, DPPH and FRAP Assay

Antioxidants ◽  
2020 ◽  
Vol 9 (4) ◽  
pp. 337 ◽  
Author(s):  
Lidija Svečnjak ◽  
Zvonimir Marijanović ◽  
Piotr Okińczyc ◽  
Piotr Marek Kuś ◽  
Igor Jerković
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Adriatic Sea ◽  
Solid Phase ◽  
Natural Antioxidants ◽  
Antioxidant Potential ◽  
Array Detector ◽  
Sea Islands ◽  
Frap Assay ◽  
Flight Mass Spectrometry

There is no systematic report about propolis chemical biodiversity from the Adriatic Sea islands affecting its antioxidant capacity. Therefore, the samples from the islands Krk, Rab, Pag, Biševo and Korčula were collected. Comprehensive methods were used to unlock their chemical biodiversity: headspace solid-phase microextraction (HS-SPME) and hydrodistillation (HD) followed by gas chromatography and mass spectrometry (GC-MS); Fourier transform mid-infrared spectroscopy (FT-MIR); ultra high performance liquid chromatography with diode array detector and quadrupole time-of-flight mass spectrometry (UHPLC-DAD-QqTOF-MS) and DPPH and FRAP assay. The volatiles variability enabled differentiation of the samples in 2 groups of Mediterranean propolis: non-poplar type (dominated by α-pinene) and polar type (characterized by cadinane type sesquiterpenes). Spectral variations (FT-MIR) associated with phenolics and other balsam-related components were significant among the samples. The UHPLC profiles allowed to track compounds related to the different botanical sources such as poplar (pinobanksin esters, esters and glycerides of phenolic acids, including prenyl derivatives), coniferous trees (labdane, abietane diterpenes) and Cistus spp. (clerodane and labdane diterpenes, methylated myricetin derivatives). The antioxidant potential determined by DPPH ranged 2.6–81.6 mg GAE/g and in FRAP assay 0.1–0.8 mmol Fe2+/g. The highest activity was observed for the samples of Populus spp. origin. The antioxidant potential and phenolic/flavonoid content was positively, significantly correlated.

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