Search results for "liquid chromatography"
showing 10 items of 942 documents
False-positive LSD testing in urine samples from intensive care patients.
1998
Unexpected positive results for lysergic acid diethylamide (LSD) were found in urine samples from 12 patients in an intensive care unit in a routine screening using the CEDIA DAU assay. None of these test results could be confirmed by high-performance liquid chromatography analysis, but all samples contained the mucolytic drug ambroxol. Further studies demonstrated that ambroxol exhibits a significant cross-reactivity in the CEDIA DAU LSD assay. Therefore, positive LSD results obtained with the CEDIA DAU assay have to be critically evaluated, particularly during the cold season, when infections of the respiratory tract often result in more frequent use of mucolytic medications.
Assays for Detection of Fungal Hallucinogens Such as Psilocybin and Psilocin
2016
Abstract Methods applicable to the detection of hallucinogenic indole compounds, namely psilocybin, psilocin, and related molecules, that have been developed so far for purposes of mycological research, toxicological studies, or forensic investigations are described in this chapter. The most current literature as well as some interesting older publications are cited, providing a historical overview of the subject. Methods of qualitative and quantitative analysis are presented. Additionally, preliminary purification steps and sample treatment before the exact quantitative determination are proposed. The methods described utilized various analytical techniques for the measurement of psilocybi…
High Pressure Processing Impact on Emerging Mycotoxins (ENNA, ENNA1, ENNB, ENNB1) Mitigation in Different Juice and Juice-Milk Matrices
2022
The aim of the present study was to investigate the potential of high-pressure processing (HPP) (600 MPa during 5 min) on emerging mycotoxins, enniatin A (ENNA), enniatin A1 (ENNA1), enniatin B (ENNB), enniatin B1 (ENNB1) reduction in different juice/milk models, and to compare it with the effect of a traditional thermal treatment (HT) (90 °C during 21 s). For this purpose, different juice models (orange juice, orange juice/milk beverage, strawberry juice, strawberry juice/milk beverage, grape juice and grape juice/milk beverage) were prepared and spiked individually with ENNA, ENNA1, ENNB and ENNB1 at a concentration of 100 µg/L. After HPP and HT treatments, ENNs were extracted from treate…
Non-Thermal Ultrasonic Extraction of Polyphenolic Compounds from Red Wine Lees
2020
This study presents the results of conventional aqueous (CE) and non-conventional ultrasound-assisted (UAE) extractions of polyphenolic compounds from lees extracts of red wine varieties (Merlot and Vranac). The effect of ultrasound extraction time (t, s), and amplitude (A,%) from a 400 W ultrasound processor with different ultrasonic probes diameters (Ds, mm) on the amount and profile of polyphenolic compounds in the obtained extracts was investigated and compared to CE. The optimal conditions resulting in maximum extraction of phenolic compounds were: Probe diameter of 22 mm, amplitude 90% and extraction time for Vranac wine lees 1500 s and for Merlot wine lees extraction time of 1361 s. …
HPLC-SEC: a new approach to characterise complex wastewater effluents
2016
ABSTRACTThis work investigates the use of HPLC-SEC to characterise dissolved organic matter (DOM) of complex wastewater effluents. A silica-based column, sodium acetate eluent and multiple detections were employed: UV-254 absorbance for humictype, and tryptophan-like (Ex/Em = 270/355) and tyrosine-like (Ex/Em = 270/310) fluorescence for protein type compounds. Effects of eluent pH, eluent ionic strength and injection volume on separation efficiency were tested. Humic-type and protein-type fractions were clearly differentiated and eluted within and out of calibration range. Eluent ionic strength had the greatest influence on global resolution; the lowest eluent concentration of 0.01 M produc…
Analysis of cannabinoids by liquid chromatography–mass spectrometry in milk, liver and hemp seed to ensure food safety
2017
A method for determining cannabinoids, Δ9-tetrahidrocannabinol (THC), 11-nor-9-carboxy-Δ9-THC (THC-COOH) and 11-hidroxy-Δ9-THC (THC-OH) in milk, liver and hemp seeds based on liquid chromatography tandem mass spectrometry has been optimized and validated. Analytes were extracted with methanol and the extracts cleaned-up by solid-phase extraction using Oasis HLB (60 mg). The developed method was validated according to the Commission Decision 2002/657/EC. The decision limit (CCα) and detection capability (CCβ) ranged from 3.10–10.5 ng g−1 and 3.52–11.5 ng g−1, the recoveries were 76–118% and matrix effect ranged from −17.8% to 19.9% in the three matrices studied. The method was applied to foo…
Amino acid profile of milk-based infant formulas
2000
The protein content and amino acid profile of three milk-based infant formulas, two of which were powdered (adapted and follow-on) and the third liquid, were determined to check their compliance with the EU directive and to evaluate whether or not they fulfil an infant's nutritional needs. To obtain the amino acid profile proteins were subjected to acid hydrolysis, prior to which the sulfur-containing amino acids were oxidized with performic acid. The amino acids were derivatized with phenylisothiocyanate (PITC) and then determined by ion-pair reverse phase high performance liquid chromatography (HPLC) In the case of tryptophan a basic hydrolysis was applied and there was no need of derivat…
Light-induced Changes in the Dimerization Interface of Bacteriophytochromes
2015
Phytochromes are dimeric photoreceptor proteins that sense red light levels in plants, fungi, and bacteria. The proteins are structurally divided into a light-sensing photosensory module consisting of PAS, GAF, and PHY domains and a signaling output module, which in bacteriophytochromes typically is a histidine kinase (HK) domain. Existing structural data suggest that two dimerization interfaces exist between the GAF and HK domains, but their functional roles remain unclear. Using mutational, biochemical, and computational analyses of the Deinococcus radiodurans phytochrome, we demonstrate that two dimerization interfaces between sister GAF and HK domains stabilize the dimer with approximat…
Application of accelerated solvent extraction followed by gel performance chromatography and high-performance liquid chromatography for the determina…
2005
Accelerated solvent extraction (ASE) has been evaluated as a fast alternative to methanolic saponification for the extraction of 12 polycyclic aromatic hydrocarbons (PAHs) from mussel tissue. Several solvent systems and different operating conditions were investigated. The mixture dichloromethane-acetone (1:1, v/v) gave the best recoveries at 125 degrees C and 1500 psi, in a total time of 10 min. No yield difference was found between freeze-drying (Fd) or drying the wet mussel with diatomaceous earth (Ded) prior to extraction. The ASE method was validated using the standard reference material SRM 2977, a freeze-dried mussel tissue with naturally present organic contaminants. The performance…
Micellar liquid Chromatographic determination of diuretics by diazotization and coupling with the Bratton-Marshall reagent
1997
Abstract A Chromatographic procedure that uses micellar mobile phases of sodium dodecyl sulphate (SDS) and propanol at pH 3 is reported for the determination, in urine samples, of thiazide diuretics (althiazide, bendroflumethiazide, chlorothiazide, hydrochlorothiazide, hydroflumethiazide, and trichloromethiazide), and other diuretics having a sulphonamide substituent in the benzene ring. Precolumn derivatization with sodium nitrite and N -(1-naphthyl)ethylenediamine, to form the coloured azo dyes of the hydrolyzed diuretics, decreased the polarity of the compounds and, consequently, their retention in the micellar eluents, and permitted detection in the visible region, eliminating thus the …