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101.
Alexandra Hütteroth Martin Jekel 《International journal of environmental analytical chemistry》2013,93(6):415-424
For the detection of unknown organic bromine compounds, a liquid chromatography–mass spectrometry (LC-MS) method with negative-ion electrospray ionization (NI-ESI) and induced in-source fragmentation (IISF) was established. After LC separation, the molecules are fragmentized in the source, and bromide is detected via m/z 79 and m/z 81 based on the isotopic occurrence of bromine. In this way, the retention times of the unknown organobromine compounds are determined, and this can be used to extract additional structural information (number of bound bromine atoms, molecular mass and fragmentation scheme) from measurements in the commonly used but less sensitive scan mode. The analysis of known organobromine compounds shows that LC/NI-ESI-IISF mass spectrometry with detection of m/z 79 and 81 is more sensitive than the detection of daughter ions (LC/ESI/MS-MS). Therefore, we present a method not only for the detection of unknown organic bromine compounds, but also for the selective and sensitive detection and quantification of known organobromine compounds. 相似文献
102.
Georgina Fortuny Laura Pineda Antoni Rúbies Francesc Centrich Ramon Companyó 《International journal of environmental analytical chemistry》2013,93(7):707-726
A method for determination of 61 organic pollutants (polycyclic aromatic hydrocarbons and organochlorine, organophosphorous and organonitrogen pesticides) is proposed. It is based on solid phase extraction (SPE) and subsequent analysis of the extract by liquid and gas chromatography coupled to tandem mass spectrometry. Method validation yielded to the following values: limits of quantification, from 0.005 to 0.020?µg?L?1; trueness, 95% to 113% and reproducibility (as percent relative standard deviation), 2% to 15%. Additionally, the method performed well in various proficiency tests. 相似文献
103.
Divya Kumar Vemuri Rambabu Gundla Naresh Konduru Ravindra Mallavarapu Naresh Kumar Katari 《Biomedical chromatography : BMC》2022,36(6):e5363
Favipiravir finished dosage was approved for emergency use in many countries to treat SARS-CoV-2 patients. A specific, accurate, linear, robust, simple, and stability-indicating HPLC method was developed and validated for the determination of degradation impurities present in favipiravir film-coated tablets. The separation of all impurities was achieved from the stationary phase (Inert sustain AQ-C18, 250 × 4.6 mm, 5-μm particle) and mobile phase. Mobile phase A contained KH2PO4 buffer (pH 2.5 ± 0.05) and acetonitrile in the ratio of 98:2 (v/v), and mobile phase B contained water and acetonitrile in the ratio of 50:50 (v/v). The chromatographic conditions were optimized as follows: flow rate, 0.7 mL/min; UV detection, 210 nm; injection volume, 20 μL; and column temperature, 33°C. The proposed method was validated per the current International Conference on Harmonization Q2 (R1) guidelines. The recovery study and linearity ranges were established from the limit of quantification to 150% optimal concentrations. The method validation results were found to be between 98.6 and 106.2% for recovery and r2 = 0.9995–0.9999 for linearity of all identified impurities. The method precision results were achieved below 5% of relative standard deviation. Forced degradation studies were performed in chemical and physical stress conditions. The compound was sensitive to chemical stress conditions. During the study, the analyte degraded and converted to unknown degradation impurities, and its molecular mass was found using the LC–MS technique and established degradation pathways supported by reaction of mechanism. The developed method was found to be suitable for routine analysis of research and development and quality control. 相似文献
104.
Eva Greibe Magnus Leth-Møller Sofie Stampe Per Ovesen Michael Pedersen Elke Hoffmann-Lücke 《Biomedical chromatography : BMC》2022,36(6):e5350
Artificial sweeteners are widely used as substitutes for sugar. The sweeteners are generally considered safe, however their whereabouts during pregnancy and lactation and the effect on child development are poorly explored. There is a need for new tools to measure these substances during pregnancy and lactation. Here, we describe the development and validation of a sensitive liquid chromatography–tandem mass spectrometry method for the simultaneous quantification of acesulfame, cyclamate, saccharin and sucralose in human plasma, umbilical cord blood, amniotic fluid and breast milk. The samples were prepared by protein precipitation and separated on a Luna Omega Polar C18 column (2.1 × 50 mm, 1.6 μm). Electrospray ionization in negative mode and multiple reaction monitoring were used to monitor the ion transitions. The validated concentration ranges were from 1 to 500 ng/ml (10–500 ng/ml for sucralose). Interassay precisions were all ≤15% and the accuracies were within ±15%. Stability, linearity, dilution integrity, carryover and recovery were also examined and satisfied the validation criteria. Finally, this analytical method was successfully applied on spiked samples of plasma, umbilical cord blood, amniotic fluid and breast milk, proving its suitability for use in clinical studies on artificial sweeteners, including during pregnancy and lactation. 相似文献
105.
Larisa Ryskalin Stefano Puglisi-Allegra Gloria Lazzeri Francesca Biagioni Carla L. Busceti Linda Balestrini Andrea Fornasiero Stefano Leone Elena Pompili Michela Ferrucci Francesco Fornai 《Molecules (Basel, Switzerland)》2021,26(9)
Curcumin (CUR), a natural polyphenol extracted from rhizome of the Curcuma longa L, has received great attention for its multiple potential health benefits as well as disease prevention. For instance, CUR protects against toxic agents acting on the human body, including the nervous system. In detail, CUR possesses, among others, strong effects as an autophagy activator. The present study indicates that CUR counteracts methamphetamine (METH) toxicity. Such a drug of abuse is toxic by disturbing the autophagy machinery. We profited from an unbiased, low variable cell context by using rat pheochromocytoma PC12 cell line. In such a system, a strong protection was exerted by CUR against METH toxicity. This was associated with increased autophagy flux, merging of autophagosomes with lysosomes and replenishment of autophagy vacuoles with LC3, which instead is moved out from the vacuoles by METH. This is expected to enable the autophagy machinery. In fact, while in METH-treated cells the autophagy substrates α-synuclein accumulates in the cytosol, CUR speeds up α-synuclein clearance. Under the effects of CUR LC3 penetrate in autophagy vacuoles to commit them to cell clearance and promotes the autophagy flux. The present data provide evidence that CUR counteracts the neurotoxic effects induced by METH by promoting autophagy. 相似文献
106.
107.
The number of chemicals with potential to reach the environment is still largely unknown, which poses great challenges for both environmental scientists and analytical chemists. Liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) is currently the instrumentation of choice for identification of wide-scope polar chemicals of concern (CECs) in water. This review critically evaluates all steps involved in screening for polar CECs in water, including sampling and extraction, analysis by LC-HRMS, data (pre-)treatment, evaluation and reporting. Passive samplers and direct injection, in combination with LC-HRMS, provide new opportunities compared with conventional grab water sampling, as do instrumental advances such as ion-mobility spectrometry coupled to HRMS (IM-HRMS). In this paper, we argue that target, suspect and non-target screening should not be viewed as three separate principles, but rather as conceptual approaches to general data treatment strategies that can be linked together. Due to the large amount of data generated, smart prioritisation strategies are needed, in particular for non-target screening, to reduce complexity and focus on data of high interest. We critically evaluate existing strategies and consider that each prioritisation step will result in data loss (as any other step in a screening study), requiring compromises depending on the research question to be tackled. Many different data treatment strategies have been developed in recent years, but structure elucidation remains a challenging and time-consuming task. We discuss current and potential future trends, e.g. effect-based methods that can be used as future prioritisation tools, technological advances like IM-HRMS and improved software solutions that can enable new data treatment strategies. 相似文献
108.
The supercritical fluid chromatography coupled with mass spectrometry (SFC‐MS) method and liquid chromatography coupled with mass spectrometry (LC‐MS) method were developed for the separation and characterization of poly (ethylene oxide) methyl glucose sesquistearate (PEO‐Glu‐sesquistearate). The products of PEO‐Glu‐sesquistearate are composed of complex oligomers. The relationship between molecular structure of these oligomers and chromatographic retention behavior in both SFC and LC were discussed and compared. As compared with LC, hydrophobic moieties of compounds favor the fast elution in SFC. The different series can be better separated by LC, while the homologues compounds in same series can be better separated by SFC, and SFC‐MS provided more comprehensive structural information. Different series such as PEO‐distearate, PEO‐stearate, PEO, PEO‐Glu‐tetrastearate, PEO‐Glu‐tristearate, PEO‐Glu‐distearate, PEO‐Glu‐stearate, and PEO‐Glu were identified by MS/MS. 相似文献
109.
Alshymaa Abdel-Rahman Gomaa Usama Ramadan Abdelmohsen Markus Krischke Martin J. Mueller Amira Samir Wanas 《Natural product research》2020,34(18):2612-2615
AbstractThe present study evaluates the chemical composition of Zinnia elegans and Gazania rigens based on their metabolomic profiles using liquid chromatography coupled with high-resolution mass spectrometry (LC‐HR-MS), alongside with the anti-infective activities of their ethanol extracts, as well as, different fractions. A significant difference was observed between the LC-MS profiles of the two plants such as, coumarins, sesquiterpene lactones and phenylethanoids which were characteristic for Z. elegans, while amides and phenolic acid derivatives were characteristic for G. rigens. These results highlight the chemical potential of Z. elegans and G. rigens. Furthermore, the ethyl acetate fraction of Z. elegans showed a significant antimalarial activity with IC50 values of 21.03 and 13.72?µg/mL against Plasmodium falciparum D6 and P. falciparum W2, respectively. 相似文献
110.
WU Yi CHU Yang ZHANG Yun-hui WU Dan GU Jing-kai 《高等学校化学研究》2007,23(4):408-411
A rapid,sensitive,and accurate method based on LC/MS/MS was developed and validated for the determination of domperidone in human plasma.Domperidone and internal standard,tramadol,were extracted from plasma with diethyl ether-dichloromethane(60∶40,volume ratio)and separated by reversed-phase HPLC with methanol-water-ammonia solution(80∶20∶0.2,volume ratio)as the mobile phase.Detection was carried out via multiple-reaction monitoring(MRM)on a Q-trapTM LC/MS/MS system(Q-trapTM).The assay result was linear over a concentration range of 0.1-30 ng/mL with a limit of quantitation(LOQ)of 0.1 ng/mL.The inter-and intra-day precision levels were within 7.52% and 12.9%,respectively,whereas the accuracy was within a range of 87.3%-114%.This method has been successfully applied to evaluate the pharmacokinetics of domperidone in Chinese healthy volunteers given an oral dose of 10 mg. 相似文献