• Hede Nguyen opublikował 1 rok, 3 miesiące temu

    of alkaloids.N-Methylation of tranexamic acid yields an unique derivative, which generates strong co-luminescence signals in the presence of an electrochemiluminescence reagent such as Ru(bpy)32+. Using this principle, we established a highly selective analytical method based on pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection for determining the tranexamic acid content in essential cosmetics. The addition of a ternary ionic association gel, Mg2+-trehalose-SiO32-, in the components of background electrolyte greatly improved the electrophoretic separation efficiency. Under the optimized assay conditions, two electrophoretic peaks attributed to the derivatives of tranexamic acid and its internal standard (sarcosine) were completely separated in 500 s, and their electrophoretic peak intensities ratio showed a good linear relationship with the initial concentration of tranexamic acid in the range of 10-750 μmol/L (correlation coefficient r2=0.9993). The limit of detection was estimated to be 3.6 μmol/L (S/N=3). Moreover, the internal standard method was further applied to the quantitative determination of tranexamic acid content in three kinds of toothpaste and two kinds of nutrient solutions in facial masks. The results showed that the average tranexamic acid content in three toothpaste samples was 4.05, 0.24, and 6.06 mg/g, while that in two facial masks was 51.3 and 7.98 mg/mL. The recoveries for the above-mentioned samples were within the range 92.5% to 104.0%, implying satisfactory results.Long-term exposure to pyrethroid insecticides is detrimental to the nervous system, reproductive system, and immune system in humans. Therefore, enrichment detection of pyrethroid pesticides is imperative. In this study, a novel carbonyl-iron powder composite silica monolithic column was first prepared for the enrichment of pyrethroid pesticide residues in tea samples. Then, the target analytes were thermally desorbed and online-injected into a gas chromatography-tandem mass spectrometry (GC-MS/MS) system. In the present method, hydroxy-terminated polydimethylsiloxane (PDMS) was covalently bonded to the surface of the SiO2 network and subsequently bonded with the carbonyl-iron powder. After the target analytes were adsorbed and concentrated in the PDMS spots, high-frequency induction heating was used for GC-MS/MS sampling. Under the optimal conditions, the detection limits of the pyrethroid pesticide residues were 3.8 to 7.5 μg/kg, and the relative standard deviation was 3.2% to 6.8% (n=6). The extraction recgh degree of automation, and good universality. This method has high significance for sample preparation and for the extraction of pesticide residues in complex matrices.At present, the kinds and the hazards of phenolic compounds in water were unclear. Research aimed at methods for the simultaneous detection of multiple phenolic compounds is still in its nascent stages. It is necessary to establish a method for the simultaneous determination of phenolic compounds in water. An analytical method was developed for the simultaneous determination of the 18 phenolic compounds in water by gas chromatography-tandem mass spectrometry (GC-MS/MS) coupled with solid phase extraction (SPE). The phenolic compounds in water were enriched and separated on an SPE column. The optimal pretreatment method was established by optimizing the chromatographic and mass spectrometric conditions. The effects of the initial pH of the water sample, type of eluting solvent, and dosage of the washing solution were investigated. Then, the 18 phenolic compounds in the water samples were determined. The optimal pretreatment extraction conditions were determined to be as followsfinal pH of water sample, 3.0; el.4 μg/L. The contents and kinds of phenolic compounds in the rivers and lakes were highest. However, the contents of phenolic compounds in the domestic water were adverse compared with the rivers and lakes, in accord with National Standard GB 8537-2008. As opposed to traditional analytical methods, the present method is characterized by simple operation without derivative or the need for anhydrous sodium sulfate for water removal, as well as high sensitivity, good stability, and reliability. The establishment of this method has important theoretical and practical significance for the development of standards and for the control of residue phenolic residue levels in water.A method combining accelerated solvent extraction (ASE) with magnetic solid-phase extraction (MSPE) and gas chromatography-mass spectrometry (GC-MS) was developed for the simultaneous detection of polycyclic aromatic hydrocarbon (PAH) and organochlorinepesticide (OCP) residues in soil samples. The analytes in the soil samples were extracted using an acetone/n-hexane (11, v/v) mixture for 5 min at 100℃. Then, the extraction pool was heated for 5 min under an extractive pressure of 11.032 MPa for three cycles. The extraction pool was washed with an acetone/n-hexane (11, v/v) mixture accounting for 60% of the pool volume, followed by nitrogen purging for 100 s. The extract was purified by MSPE using self-made magnetic ZIF-8/nZVI materials at room temperature. The analytes were detected by GC-MS/MS. Under the optimized conditions, good linearities were obtained for the 16 PAHs and the 23 OCPs in the range of 5-200 μg/kg, with correlation coefficients (r2) above 0.99. The limits of detection (LODs) were 0.04-1.21 μg/kg. At three spiked levels in the soil samples, the recoveries of the 39 analytes were between 63.9% and 112.1%, with relative standard deviations (RSDs) between 0.4% and 26.2%. The method was demonstrated to be successful for the determination of 16 PAH and 23 OCP residues in soil samples, with good recoveries.Silica monolith particles with sizes of 2-5 μm and pore sizes of 20-60 nm were obtained by grinding, flotation, pseudomorphic transformation, and hydrothermal treatment of the silica monolith prepared by the sol-gel method. The pseudomorphic transformation was performed with a dual micellar templating system consisting of Capstone FS-66, a partially fluorinated anion surfactant, and cetyltrimethylammonium bromide (CTAB), a commonly used cation surfactant. Hydrothermal treatment with a sodium carbonate solution was adopted to further expand the pore size. Scanning electron microscopy (SEM) images and N2 adsorption-desorption isotherm measurement results of the silica monolith particles before and after the treatments clearly demonstrated the changes in morphology caused by these treatments. Afterward, a long-chain polyethylene glycol (PEG) containing silane was bonded on the surface of the as-prepared particles, and the resulting products were characterized by elemental analysis and FT-IR spectroscopy analysis, and evaluated by high performance liquid chromatography (HPLC). Elemental analysis and thermogravimetric analysis (TGA) of the bonded stationary phase revealed that the bonding amount of PEG on the silica surface is about 8%. It has been shown that silica monolith particles can be treated and modified for the separation of proteins in size exclusion chromatography mode. It is also demonstrated that the bonded stationary phase can be used for the separation of ribonuclease A and lysozyme in hydrophobic interaction chromatography mode, and for the separation of highly polar compounds (picolinic acid, levodopa, melamine, and catechol) in hydrophilic interaction chromatography mode. The results indicate the versatility of the PEG-bonded stationary phase and its promising application to multi-modal separation in HPLC.A novel sensitive method for the determination of the five primary metabolites of phthalate esters (PAEs) in urine was developed by combining dispersive liquid-liquid microextraction (DLLME) using ionic liquids with high performance liquid chromatography (HPLC). The factors affecting the efficiency of DLLME were optimized. The types and proportions of extraction solvent and dispersants, as well the ultrasonic extraction time, cooling time, and centrifugal time, were determined. The optimal conditions were as followsextraction solvent[C8MIM]PF6] 35 μL; dispersants[BSO3HMIm]OTf] 30 μL,[C4MIM]BF6] 120 μL; NH4PF6 0.1 g, extraction at 35℃, ultrasonic dispersion for 5 min, cooling in ice water for 5 min, centrifugation at 4000 r/min for 5 min. After optimization, the five primary metabolites of PAEs were determined. The method showed a good linear relationship within the concentration range of 0.5-1000 μg/L. The determination coefficients (R2) were greater than 0.9955. The detection limit was in the range of 0.16-0.19 μg/L. Under the optimized conditions, the extraction recoveries for the PAEs were 92.9%-105.0%, and the relative standard deviations (RSDs) of the intra- and inter-day precisions were less then 5.96%. Urine samples collected from 10 diabetic patients were tested, and the exposure level of the population to the PAE metabolites was evaluated. All the PAE metabolites were detected in these samples, and the detection rate of 2-ethylhexyl hydrogen phthalate (MEHP) was 100%. In conclusion, no toxic organic reagents were added during the extraction process in this method, and multifunctional ionic liquids were used as the extraction agent, dispersant, and salting-out agent. In other words, the extraction process was demonstrated to be green, simple, and efficient. The developed method has high sensitivity and stability, and it is suitable for the determination of trace PAE metabolites in human urine.Using o-phthalaldehyde (OPA) as the derivatization reagent, a precolumn derivatized -high performance liquid chromatography (HPLC) method was developed for the simultaneous determination of amino acid neurotransmitters taurine (Tau), glutamic acid (Glu), glycine(Gly), and γ -aminobutyric acid (γ-GABA), as well as the monoamine neurotransmitter dopamine (DA), in serum samples. The samples and ethanol were mixed at a volume ratio of 12 (v/v) for protein precipitation. After centrifugation, the supernatant was withdrawn and blown to dryness using nitrogen. The residue was pre-column derivatized with OPA, and the derivatized product was isolated by gradient elution ona Luna 5u C18 column (250 mm×4.6 mm, 5 μm). Under the optimal experimental conditions, the five neurotransmitters showed good linearities (r2 ≥ 0.9866). The limits of detection were between 0.10 and 0.40 μmol/L. The spiked recoveries at different spiked levels were 87.57%-115.31%, and the RSDs were below 7.80%. This method is simple, sensitive, and it can be promised for the simultaneous detection of amino acid and monoamine neurotransmitters.Archaea are single-cell microorganisms, structurally and biochemically similar to bacteria and fungi. Most of them live in extreme environments, such as high salt, extremely acidic, extremely hot, and anaerobicenvironments. The membrane structure and related metabolic pathways of archaea are different from those of other microorganisms. Therefore, studying the lipid metabolism of archaea is of great significance for exploring the life activities in extreme environments. As the first step in lipidomic analysis, lipid extraction and pretreatment methods play an important role, as they influence the accuracy and reliability of the final results. We harnessed ultra-performance liquid chromatography coupled with high-resolution mass spectrometry (UPLC-HRMS) to detect the total normal lipids. The hyperthermophilic archaeon Pyrococcus yayanosii was selected as the model. The Bligh-Dyer acidic method, Folch method, methyl tert-butyl ether (MTBE) method, and solid-phase extraction (SPE) method were compared by multi-component analysis in terms of extraction efficiency, reproducibility, and extraction discrimination.

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