Search results for "liquid chromatography"
showing 10 items of 942 documents
New method for determination of ochratoxin A in beer using zinc acetate and solid-phase extraction silica cartridges
2006
Abstract A new method for the determination of ochratoxin A (OTA) in beer has been developed. The new method has been compared with a reference method currently accepted as AOAC official first action. The limits of detection and quantification of the proposed method were 0.0008 and 0.0025 ng/ml, respectively, while they were 0.0025 and 0.0075 ng/ml, respectively, in the AOAC method used as reference. The recovery levels in the 0.025–0.40 ng OTA/ml spiking range for the proposed and the reference methods were 80.6–87.6% and 78.2–83.8%, respectively. The relative standard deviations of recoveries were 2.6–7.5% for the proposed method and 0.7–6.1% for the reference method. Passing and Bablok r…
Simultaneous analysis of twenty-six mycotoxins in durum wheat grain from Italy
2016
Abstract A multi-mycotoxin analysis method based on liquid chromatography coupled to triple quadrupole mass spectrometry was validated and applied for the determination of twenty-six mycotoxins, including eight trichothecenes, three fumonisins, sterigmatocystin, ochratoxin A, four aflatoxins, zearalenone, five “emerging” mycotoxins and three Alternaria mycotoxins in 74 durum wheat samples from central Italy. Eighty-eight percent of the analysed samples contained one or more mycotoxins, with enniatin B showing the highest contamination levels (78% of samples with levels ranging from 23 to 1826 ng/g), followed by enniatin B1 (10–1384 ng/g) and deoxynivalenol (48–2267 ng/g). This work gives an…
Multimycotoxin analysis in water and fish plasma by liquid chromatography-tandem mass spectrometry
2015
High performance liquid chromatography-mass spectrometry was used for the determination of 15 mycotoxins in water and fish plasma samples, including aflatoxins, fumonisins, ochratoxin A, sterigmatocistin, fusarenon-X and emerging Fusarium mycotoxins. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a sample treatment for the simultaneous extraction of mycotoxins. Results showed differences in recovery assays when different extraction solvents were employed. Ethyl acetate showed better recoveries for the major part of mycotoxins analyzed, except for aflatoxins B2, G1 and G2, which showed better recoveries when employing chloroform as extractant solvent. Fumonisi…
Improved sensitivity of ochratoxin A analysis in coffee using high-performance liquid chromatography with hybrid triple quadrupole-linear ion trap ma…
2016
A novel and sensitive method utilising high-performance liquid chromatography coupled to triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS) was developed in order to analyse the content of ochratoxin A (OTA) in coffee samples. The introduction of the triple-stage MS scanning mode (MS(3)) has been shown to increase greatly sensitivity and selectivity by eliminating the high chromatographic baseline caused by interference of complex coffee matrices. The analysis included the sample preparation procedure involving extraction of OTA using a methanol-water mixture and clean-up by immunoaffinity columns and detection using the MS(3) scanning mode of LC-QqQLIT-MS/MS. The propose…
Influence of roasting and different brewing processes on ochratoxin A content in coffee determined by high-performance liquid chromatography-fluoresc…
2008
A rapid and reliable procedure has been developed for the determination of ochratoxin A (OTA) in green and roasted coffee. The method consists of extraction of the sample with methanol-5% aqueous sodium hydrogen carbonate/1% PEG8000 (20:80), followed by immunoaffinity column (IAC) clean-up and, finally, high-performance liquid chromatography (HPLC) determination with fluorimetric detection. Mean recoveries for green and roasted coffee spiked at different levels ranging from 94 and 105% were obtained. The limit of determination (S/N = 3) was 0.032 ng g(-1) and the precision (within-laboratory relative standard deviation) was 6%. The method described has been used to assess the influence of r…
Synthesis and evaluation of fluorine-18 labeled glyburide analogs as β-cell imaging agents
2003
Glyburide is a prescribed hypoglycemic drug for the treatment of type 2 diabetic patients. We have synthesized two of its analogs, namely N-[4-[beta-(2-(2'-fluoroethoxy)-5-chlorobenzenecarboxamido)ethyl]benzenesulfonyl]-N'-cyclohexylurea (2-fluoroethoxyglyburide, 8b) and N-[4-[beta-(2-(2'-fluoroethoxy)-5-iodobenzenecarboxamido)ethyl]benzenesulfonyl]-N'-cyclohexylurea (2-fluoroethoxy-5-deschloro-5-iodoglyburide, 8a), and their fluorine-18 labeled analogs as beta-cell imaging agents. Both F-18 labeled compound 8a and compound 8b were synthesized by alkylation of the corresponding multistep synthesized hydroxy precursor 4a and 4b with 2-[(18)F]fluoroethyl tosylate in DMSO at 120 degrees C for …
Radiosynthesis of 1-(4-(2-[18F]fluoroethoxy)benzenesulfonyl)-3-butyl urea: a potentialβ-cell imaging agent
2002
Summary Tolbutamide (1) is a sulfonurea agent used to stimulate insulin secretion in type 2 diabetic patients. Its analogue 1-(4-(2-[ 18 F]fluoroethoxy)benzenesulfonyl)-3butyl urea (3) was synthesized in overall radiochemical yields of 45% as a potential b-cell imaging agent. Compound 3 was synthesized by 18 F-fluoroalkylation of the corresponding hydroxy precursor (2 )w ith 2-[ 18 F]fluoroethyltosylate in DMF at 1208C for 10 min followed by purification with HPLC in a synthesis time of 50 min. Insulin secretion experiments of the authentic 19 F-standard compound on rat islets showed that the compound has a similar stimulating effect on insulin secretion as that of tolbutamide (1). The part…
Micellar versus hydro-organic mobile phases for retention-hydrophobicity relationship studies with ionizable diuretics and an anionic surfactant
2004
Abstract Logarithm of retention factors (log k ) of a group of 14 ionizable diuretics were correlated with the molecular (log P o/w ) and apparent (log P app ) octanol–water partition coefficients. The compounds were chromatographed using aqueous–organic (reversed-phase liquid chromatography, RPLC) and micellar–organic mobile phases (micellar liquid chromatography, MLC) with the anionic surfactant sodium dodecyl sulfate (SDS), in the pH range 3–7, and a conventional octadecylsilane column. Acetonitrile was used as the organic modifier in both modes. The quality of the correlations obtained for log P app at varying ionization degree confirms that this correction is required in the aqueou…
Quantification of rifampicin and rifabutin in plasma of tuberculosis patients by micellar liquid chromatography
2020
A Micellar Liquid Chromatographic method is described to determine Rifampicin and Rifabutin in plasma from Tuberculosis patients. Samples were diluted in mobile phase and then directly injected, avoiding long and tedious extraction steps. The analytes were resolved from the matrix without interferences from endogenous compounds using a mobile phase of sodium dodecyl sulfate 0.15 mol L-1–6%(v/v) 1-pentanol and phosphate buffer at pH 3, running at 1 mL min−1 through a C18 column at 25 °C. Detection was carried out by UV absorbance at 270 nm. Under these conditions, the final chromatographic analysis time was 22 min. The analytical methodology was validated following the FDA 2018 Bioanalytical…
Incorporation of metal-organic framework amino-modified MIL-101 into glycidyl methacrylate monoliths for nano LC separation.
2018
Metal-organic frameworks consisting of amino-modified MIL-101(M: Cr, Al, and Fe) crystals have been synthesized and subsequently incorporated to glycidyl methacrylate monoliths to develop novel stationary phases for nano-liquid chromatography. Two incorporation approaches of these materials in monoliths were explored. The metal-organic framework materials were firstly attached to the pore surface through reaction of epoxy groups present in the parent glycidyl methacrylate-based monolith. Alternatively, NH2 -MIL-101(M) were admixed in the polymerization mixture. Using short time UV-initiated polymerization, monolithic beds with homogenously dispersed metal-organic frameworks were obtained. T…