Littérature scientifique sur le sujet « SPE-HPLC-MS/MS »
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Articles de revues sur le sujet "SPE-HPLC-MS/MS"
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Chen, Kun-Ming, Ana Calcagnotto, Junjia Zhu, Yuan-Wan Sun, Karam El-Bayoumy et John P. Richie Jr. « Comparison of an HPLC-MS/MS Method with Multiple Commercial ELISA Kits on the Determination of Levels of 8-oxo-7,8-Dihydro-2'-Deoxyguanosine in Human Urine ». Journal of New Developments in Chemistry 2, no 2 (16 décembre 2018) : 1–13. http://dx.doi.org/10.14302/issn.2377-2549.jndc-18-2430.
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Introduction: Analysis of 8-oxodG is usually conducted by either chromatography-based methods or by immunochemical methods commonly used based upon their low cost and high-throughput. However, concern regarding the accuracy of ELISA methods has complicated their use. We directly compare the levels of urinary 8-oxodG obtained by HPLC-MS/MS with three commercially available ELISA kits in this report. Methods: In the current study, a total of 9 human urine samples were analyzed by LC-MS/MS and three commonly used commercial available ELISA kits. Results: We found that urinary 8-oxodG levels analyzed by HPLC-MS/MS [1.4 ± 0.3 nmol/mmol creatinine) were 7.6- to 23.5-fold lower than those detected by ELISA. Overall, the correlations between ELISA and HPLC-MS/MS were poor but were improved after SPE purification for kits from ENZO (P = 0.2817 without SPE; P = 0.0086 with SPE) and Abcam (P = 0.0596 without SPE; P = 0.0473 with SPE). Discussion and conclusion: While we confirmed that SPE purification can improve the correlation between the selected ELISA kits and HPLC-MS/MS, HPLC-MS/MS is still the method of choice to accurately assess the levels of 8-oxodG in human urine.
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Pang, Guo-Fang, Chun-Lin Fan, Feng Zhang, Yan Li, Qiao-Ying Chang, Yan-Zhong Cao, Yong-Ming Liu et al. « High-Throughput GC/MS and HPLC/MS/MS Techniques for the Multiclass, Multiresidue Determination of 653 Pesticides and Chemical Pollutants in Tea ». Journal of AOAC INTERNATIONAL 94, no 4 (1 juillet 2011) : 1253–96. http://dx.doi.org/10.1093/jaoac/94.4.1253.
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Abstract An effcient and sensitive method has been established for simultaneous determination of 653 pesticides in teas by GC/MS and HPLC/MS/MS. The method involved extraction with acetonitrile followed by cleanup using Cleanert-TPT SPE and subsequent identifcation and quantitation of 490 pesticides by GC/MS and 448 pesticides by HPLC/MS/MS. The LODs for pesticides determined by GC/MS were between 1.0 and 500 µg/kg, and those determined by HPLC/MS/MS were between 0.03 and 4820 µg/kg. At the low fortifcation levels of 0.01–100 µg/kg, the average recoveries of 94% of the pesticides determined by GC/MS were between 60 and 120%, 77% of which had an RSD below 20%. For 91% of pesticides determined by HPLC/MS/MS, the average recoveries were between 60 and 120%, 76% of which had an RSD below 20%. The paper also reports a novel SPE column, Cleanert TPT, which comprised graphitized carbon black (PestiCarb), polyamine silica, and amide polystyrene for purifying the tea samples. The results indicated good repeatiblity and reproducibility.
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Miao, Hong-Hao, Yi-Nan Wang, Ru-Song Zhao, Wei-Lin Guo, Xia Wang, Ting-Ting Shen, Chen Wang et Xi-Kui Wang. « Determination of triclocarban in aquatic plants by using SPE combined with HPLC-ESI-MS/MS ». Anal. Methods 6, no 7 (2014) : 2227–32. http://dx.doi.org/10.1039/c3ay42304b.
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A convenient and reliable analytical method was developed for determination of antibacterial triclocarban in aquatic plants based on homogenate extraction, SPE clean-up, and HPLC-ESI-MS/MS determination.
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Kovalczuk, T., J. Poustka et J. Hajšlová. « HPLC-MS/MS method for analysis of isoproturon in difficult matrix : poppy seeds ». Czech Journal of Food Sciences 26, No. 2 (17 avril 2008) : 146–52. http://dx.doi.org/10.17221/2469-cjfs.
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While several validated methods have been developed for analysis of phenylurea herbicides in staple food plants, analytical procedures suitable for their quantification in minor crops such as poppy seeds are not available. For the registration of isoproturon use in this crop, the documentation of dynamics of its residues following treatment was requested. To accomplish this task, HPLC-MS/MS method was developed. Extraction of residues was realised by methanol-water mixture, Supelclean LC-18 SPE cartridges were used for purification of crude extracts. For HPLC separation of isoproturon SPE fraction Lichrospher C18 column (25 cm × 4 mm, 5 μm) was employed. For detection and quantification of target analyte, mass spectrometer with ion trap analyser operated in positive atmospheric pressure chemical ionisation (APCI) and MS/MS mode was used. Following performance parameters of method were obtained: detection limit 0.01 mg/kg, recovery 84%, and repeatability 7%.
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Sturm, Sonja, Christina Högner, Christoph Seger et Hermann Stuppner. « Combining HPLC-DAD-QTOF-MS and HPLC-SPE-NMR to Monitor In Vitro Vitetrifolin D Phase I and II Metabolism ». Metabolites 11, no 8 (9 août 2021) : 529. http://dx.doi.org/10.3390/metabo11080529.
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By combining HPLC-DAD-QTOF-MS and HPLC-SPE-NMR, the in vitro metabolism of vitetrifolin D, a pharmacologically active key molecule from Vitex agnus-castus in liver cell fractions, was investigated. Twenty-seven phase I and phase II metabolites were tentatively identified from the culture broth by HPLC-DAD-QTOF-MS. The subsequent HPLC-SPE-NMR analysis allowed for the unequivocal structural characterization of nine phase I metabolites. Since the preparative isolation of the metabolites was avoided, the substance input was much lower than in conventional strategies. The study did prove that the use of hyphenated instrumental analysis methodologies allows for the successful performance of in vitro metabolism studies, even if the availability of substances is very limited.
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Liu, Lei, Yabin Wen, Kangning Liu, Liang Sun, Yaxin Lu et Zheng Yin. « Simultaneous determination of a broad range of cardiovascular drugs in plasma with a simple and efficient extraction/clean up procedure and chromatography-mass spectrometry analysis ». RSC Adv. 4, no 38 (2014) : 19629–39. http://dx.doi.org/10.1039/c4ra01045k.
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A simple, easy to use and efficient method was described for simultaneous determination of ten cardiovascular drugs with a broad range of physicochemical properties in rat plasma via online SPE and HPLC-MS/MS.
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Sun, Xiaojie, Yuanhao Yang, Qiangbing Tian, Derong Shang, Jun Xing et Yuxiu Zhai. « Determination of gentamicin C components in fish tissues through SPE-Hypercarb-HPLC-MS/MS ». Journal of Chromatography B 1093-1094 (septembre 2018) : 167–73. http://dx.doi.org/10.1016/j.jchromb.2018.07.011.
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Wang, Bo, Jianyu Liu, Xia Zhao, Kaizhou Xie, Zhixiang Diao, Genxi Zhang, Tao Zhang et Guojun Dai. « Determination of Eight Coccidiostats in Eggs by Liquid–Liquid Extraction–Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry ». Molecules 25, no 4 (22 février 2020) : 987. http://dx.doi.org/10.3390/molecules25040987.
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A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs.
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Nurfadhila, Lina, Marsah Rahmawati, Nur Komala Fitri, Salsabila Granadha Nibullah et Welly Windari. « Analisis senyawa acetaminophen dalam sampel biologis dengan berbagai macam metode ». Journal of Pharmaceutical and Sciences 6, no 3 (27 juillet 2023) : 1221–37. http://dx.doi.org/10.36490/journal-jps.com.v6i3.197.
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Acetaminophen atau Paracetamol merupakan senyawa yang memiliki efek farmakologi sebagai analgesik dan antipiretik. Tujuan dari review jurnal ini yaitu guna mengetahui serta memahami berbagai macam metode yang bisa digunakan untuk menganalisis sampel biologis pasien ketika mengkonsumsi paracetamol melalui sampel biologisnya. Proses awal untuk melakukan analisis yaitu dengan melakukan preparasi sampel, sampel-sampel dipreparasi dengan berbagai macam metode yang sesuai seperti, metode ekstraksi cair-cair, ekstraksi fase padat (solid phase extraction (SPE) dan metode presipitasi protein, selanjutnya sampel tersebut akan dianalisis menggunakan instrumen yang tepat seperti, GC-MS, LLE, LC-MS, HPLC-MS, ataupun UHPLC-MS. Dari beberapa instrumen yang digunakan metode HPLC-MS merupakan metode yang paling efektif untuk melakukan analisis sampel biologi, karena HPLC-MS dinilai cepat, selektif dan sensitif serta memiliki LLOQ atau nilai batas bawah kuantifikasi yang paling rendah.
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Wang, Xiaoli, Tao Guo, Yunbo Wei, Guiju Xu, Na Li, Jinhong Feng et Rusong Zhao. « Determination of Quinolone Antibiotic Residues in Human Serum and Urine Using High-Performance Liquid Chromatography/Tandem Mass Spectrometry ». Journal of Analytical Toxicology 43, no 7 (16 mai 2019) : 579–86. http://dx.doi.org/10.1093/jat/bkz034.
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Abstract Quinolone antibiotic residues may pose potential threat to human health. A rapid and sensitive method was developed for the determination of quinolone residues in human serum and urine. After solid phase extraction (SPE) process, eight quinolone residues were analyzed by high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) using ciprofloxacin-d8 as the internal standard. The relative standard deviation of intra-day and inter-day precision for the eight quinolones were less than 7.52% and the accuracies ranged from 95.8% to 103% in human serum, and from 94.1% to 104% in human urine. The extraction recoveries for the eight quinolones varied from 80.2% to 113% in human serum and 83.4% to 117% in human urine. The limit of detection for the eight quinolones was 0.50–1.00 ng/mL. Quinolone antibiotic residues in human serum and urine from 12 volunteers were successfully analyzed with the validated method. The SPE-HPLC-MS/MS method was useful for accurate determination of quinolone antibiotic residues in human body.
Thèses sur le sujet "SPE-HPLC-MS/MS"
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Brown, Stacy D., Fessou Lawson-Hellu, Derek Murrell et Sam Harirforoosh. « Simultaneous Determination of Five Antiretroviral Drugs Plus Cobicistat in Human Plasma Using Strong Cation Mixed-Mode SPE and HPLC-MS/MS ». Digital Commons @ East Tennessee State University, 2017. https://dc.etsu.edu/etsu-works/5268.
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Figueiredo, Natália Guimarães de. « Avaliação da remoção de interferentes endócrinos, ativos farmacêuticos e cafeína em água para abastecimento público do estado de São Paulo ». Universidade de São Paulo, 2014. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-02102014-140733/.
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Alguns compostos orgânicos como interferentes endócrinos e ativos farmacêuticos estão sendo encontrados em águas superficiais e vêm chamando a atenção de orgãos públicos e da comunidade científica. Dentre esses compostos, foram enfatizados nesse trabalho, o hormônio sintético 17α-etinilestradiol, o surfactante (4-nonilfenol), bisfenol A, o antibiótico β-lactâmico amoxicilina e a cafeína como traçador de atividade antrópica. Estes compostos são continuamente introduzidos em corpos d\'água pelo lançamento de esgoto in natura o que afeta a qualidade da água, a saúde dos ecossistemas e impacta o suprimento de água potável. Considerando a baixa taxa de remoção desses contaminantes pelo tratamento de água atualmente utilizado no Brasil e o estado de degradação dos mananciais de água para abastecimento público, esse trabalho apresenta o desenvolvimento de metodologia analítica para determinação dos compostos citados e a avaliação da eficiência de remoção quando o tratamento convencional de água é aplicado. A determinação foi baseada em métodos já estabelecidos e envolveram as etapas de limpeza e concentração de amostra usando extração em fase sólida (SPE) e análise por cromatografia a líquido de alta eficiência (HPLC) com detector de arranjo de diodos (DAD) e espectrometria de massas. As amostras do Reservatório do Guarapiranga foram utilizadas para ensaios em escala laboratorial que simulavam o tratamento convencional de água em planta real. Os resultados mostraram a adequação dos métodos utilizados para a separação e determinação desses compostos em amostras ambientais. Além disso, apontaram para a necessidade de se avaliar a utilização de metodologias não convencionais que otimizem a remoção pelo tratamento de água atualmente utilizado.Some organic compounds, such as endocrine disruptors and pharmaceuticals, are being found in the surface water, and are concerning both the public organs and the scientific community. Among these compounds, the synthetic hormone 17α-ethinylestradiol, the surfactant (4-nonylphenol), bisphenol-A, the β-lactam antibiotic amoxicillin and the marker of human activity caffeine were highlighted in the present work. These compounds are continuously drained to the water bodies by sewers, affecting not only the water quality itself, but also the ecosystems, and impacting the drinking water availability. Currently in Brazil, the removal rate of these contaminants is low, whereas the water sources for public supply are highly degraded. In this context, the present work develops an analytical method to detect the aforementioned compounds, and to evaluate the efficiency of its removal by conventional water treatments. Detection was based on pre-established methods and steps involved clean up and samples concentration by solid phase extraction (SPE), high performance liquid chromatography with diode array detection (DAD), and mass spectrometry. Recovery tests were done using environmental samples from Guarapiranga Reservoir (São Paulo, SP). This samples were further used in laboratorial tests, simulating real scale water conventional treatments. Current results revealed the adequacy of the chosen methods in the separation and determination of the abovementioned compounds from natural samples. Also, they highlight the need for the evaluation of non-conventional methodologies that optimize removal by current water treatment.
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Gru, Yvan. « Couplage avancé de type HPLC avec préconcentration en ligne et spectrométrie de masse (SPE-LC/MS/MS) : identification et quantification de micropolluants organiques dans les eaux : effets de la matrice ». Rennes 1, 2010. http://www.theses.fr/2010REN1S020.
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De nombreux composés d’origine anthropique sont détectés dans l’environnement, particulièrement dans les eaux de surface utilisées comme ressource. Parmi ces molécules, les pesticides, bien qu’ils soient parfois présents à de très faibles concentrations, peuvent causer des dommages sanitaires ou environnementaux. La préparation de l’échantillon et la méthode de détection sont les deux points critiques de la qualité du dosage de tels substances dans les eaux. L’extraction demeure notamment une étape fastidieuse qui génère des problèmes de récupération. Pour les réduire, une technique de chromatographie liquide avec préconcentration en ligne (SPE-LC) couplée à un spectromètre de masse de type piège ionique linéaire (LIT) a été développée et validée en matrice eau propre (type eau d’Evian) et en eau de rivière (type rivière Loire - Nantes). Les critères de performances retenus étaient les suivants : exactitude, reproductibilité, sélectivité et sensibilité afin d’atteindre aisément des limites de quantification (LQ) au niveau 10 ng/L, pour un grand nombre de molécules. Près de 210 pesticides sont analysés dans le même run chromatographique en mode ElectroSpray positif. 2 ml d’échantillon d’eau sont percolés à travers une cartouche appropriée. Les LQ atteintes dans les deux matrices sont, pour la plupart des molécules inférieures ou égales à 10 ng/L. Les résultats montrent que la SPE-LC couplée à la spectrométrie de masse en tandem (MS/MS) est une technique adaptée, entièrement automatisable, pour réaliser une analyse multi-résidus de routine dans ces types d’eaux. La dégradation des molécules a par la suite été étudiée par la recherche de quelques métabolites, et aussi par la modification des conditions de stockage, montrant ainsi l’importance d’évaluer la stabilité des composés en milieu aqueux (hydrolyse, photolyse). L’étude s’est ensuite focalisée sur la qualité d’identification des composés par l’utilisation du mode d’acquisition MRM-EPI (Full scan MS/MS) disponible sur ce type de spectromètre. Ce mode de balayage se révèle comme un outil de choix pour assurer l’identification en dosage multi-résidus. Enfin, le thème d’effet matrice a été largement abordé, car la technique développée donnait lieu à des suppressions de signal non négligeables pour un certain nombre de composés (exaltations de signal plus rarement). L’origine de ces effets matrice a été évaluée par des essais d’introduction post-colonne, montrant que l’ionisation par Electrospray est un point critique. Il a fallu apporter des solutions à la maîtrise et à la réduction de ces effets incommodants pour la restitution juste d’une concentration d’un analyte présent dans un échantillon d’eau. L’étalonnage interne s’est montré efficace et ainsi a été choisi, par application ou non d’un étalon interne adapté pour une molécule préciseTo analyze swiftly and reliably numerous pesticides in waters, an on-line solid phase extraction liquid chromatography technique (on-line SPE-HPLC) coupled with triple quadripole linear ion trap mass spectrometry (Q-Trap MS/MS) procedure was developed for a large range of chemical families with detection limits at the 10 ng/L level. In this study, triazines, phenylureas, organophosphorus compounds and others (near than 210 compounds) were tested in the same ESI positive chromatographic run (less than 25 min). 2 ml of water sample (filtered if necessary) were injected into the SPE-HPLC system through a preconcentration cartridge. Analytes were eluted by a suitable mobile phase towards an analytical column (monolithic stationary phase), then detected and quantified by the mass spectrometer (MS/MS). The LOQ were achieved under the 10 ng/L level for the most of compounds in the both matrices (tap water and river water). Degradation of molecules was studied by research of few metabolites, and also by modification of storage conditions, showing the importance to evaluate stability of compounds in aqueous environment (hydrolysis, photolysis). The study was then focused on the identification by using the MRM-EPI scan mode (Full scan MS/MS), available on this kind of mass spectrometer. Results show that on-line-SPE-LC technique, coupled with hybrid triple quadripole linear ion trap mass spectrometry is a suitable way to determine multiple organic residues in waters. Finally, matrix effects theme was largely approached, since developed technique gave place non negligible signal suppressions for few compounds (signal enhancement more rarely). Matrix effects origin was evaluated by post-column introductions tests, showing that Electrospray ionization is a critical point. It was necessary to bring solutions of the control and the reduction of these annoying effects in the just restoration of an analyte concentration. The internal calibration showed effective and so was chosen, by application or not of an internal standard adapted for a particular molecule
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Čáková, Veronika. « Contribution à l'étude phytochimique d'orchidées tropicales : identification des constituants d'Aerides rosea et d'Acampe rigida : techniques analytiques et préparatives appliquées à Vanda coerulea et Vanda teres ». Phd thesis, Université de Strasbourg, 2013. http://tel.archives-ouvertes.fr/tel-00997451.
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L'analyse de la composition chimique de deux orchidées de la sous-tribu des Aeridinae, Aerides rosea Lodd. ex. Lindl. & Paxton et Acampe rigida (Buch.-Ham. ex Sm.) P. F. Hunt, a été menée en ayant recours à des techniques de couplages et grâce à une stratégie de déréplication. Dix dérivés phénanthréniques ont ainsi été identifiés dans les tiges d'A. rosea, dont deux nouvellement décrits. Quatre stilbénoïdes, trois dérivés d'acides phénoliques et quatre esters d'acide cinnamique ont été identifiés dans les tiges d'A. rigida. Nous avons également effectué des dosages de traceurs dans différents échantillons de deux représentants de la tribu des Vandeae : Vanda teres (Roxb.) Lindl. et Vanda coerulea Griff. ex. Lindl., afin de mettre en évidence d'éventuelles variations de composition en fonction des facteurs environnementaux et du stade de croissance végétative. Enfin, nous avons mis au point des conditions d'isolement préparatif par chromatographie de partage centrifuge afin de purifier des marqueurs biologiques préalablement identifiés dans les tiges de Vanda teres : trois glucospyranosyloxybenzyl - malates ainsi que leur précurseur biosynthétique.
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Alves, Filho Elenilson de Godoy. « Análises de compostos orgânicos não específicos no esgoto sanitário doméstico através das técnicas RMNq e HPLC-(UV/MS)-SPE-ASS-NMR ». Universidade Federal de São Carlos, 2014. https://repositorio.ufscar.br/handle/ufscar/6338.
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Previous issue date: 2014-10-10Universidade Federal de Sao Carlos
The growth of industrial deployment and urbanization play a major role in the degradation of global environmental and resource depletion mainly in countries in development such as Brazil. The problems regarding water pollution in Latin America have been well-documented, and there is no evidence of substantive effort to change the situation. There are a large number of organic pollutants that leads several damages to the ecosystem, threatening human health and are flushed to wastewater treatment plants (WWTPs). The WWTPs are responsible for the removal of natural and anthropogenic pollutants from the sewage and, for this, play an important role in protection of human health and the environment. Due to the varying operational conditions, process and quality, the wastewater treatments need to be monitored continuously to ensure a reliable and efficient operation. Therefore, the NMR analyses are widely used in the study of different components of wastewater such as complex organic matter (fulvic and humic acids), sludge and organic contaminants. In the present work, we employed two methods to study wastewater samples: non-targeted 1D (13C and 1H) and 2D NMR spectroscopy analyses to characterize the largest possible number of compounds in urban wastewater; and analysis by HPLC-(UV/MS)-SPE-ASS-NMR to detect and elucidate the non-specific recalcitrant in treated wastewater, sparing the common use of standards. In the non-targeted 1D NMR analysis, we employed also a method to study wastewater samples by chemometric and quantitative analyses to monitor the seasonal variations and identify anomalous discharges in urban wastewater system. The set of data were constituted of several compounds on which the concentration ranges considerably with treatment and seasonality. An anomalous discharge, the influence of storm water on the wastewater composition and recalcitrant compounds (LAS surfactant homologues) in the effluent were further identified. The seasonal variations and abnormality in the composition of organic compounds in sewage indicated that the employed procedure can be useful to identify the pollution source, to follow up the efficiency of WWTPs plants to design preventive actions in order to protect equipment and preserve the environment.
Atualmente, o crescimento industrial, a urbanização e as atividades rurais, como a agricultura, são um dos responsáveis pela deterioração do meio ambiente, principalmente nos países em desenvolvimento, como o Brasil. Problemas relacionados com a poluição das águas fluviais na América Latina têm sido bem documentados, porém não há evidências de esforços substanciais para alterar essa situação. Existem vários poluentes orgânicos presentes no esgoto tratado pelas Estações de Tratamento de Esgoto (ETEs) que podem causar danos aos ecossistemas e, com isso, ameaçar a saúde humana. As ETEs são responsáveis pela remoção da maioria dos poluentes antropogênicos ou naturais presentes no esgoto sanitário doméstico, e por isso, desempenham um papel fundamental na preservação do meio ambiente e consequentemente da saúde pública. Devido às variações das condições operacionais, processos e qualidade dos descartes, o tratamento do esgoto sanitário doméstico precisa ser monitorado continuamente para assegurar eficiência operacional. Para o estudo de contaminações ambientais, a RMN tem-se configurado como uma valiosa ferramenta, uma vez que ela tem contribuído significativamente no estudo de componentes químicos presentes nas águas e no lodo de esgoto; nas análises de interações com as substâncias húmicas e fúlvicas, além de contaminações ambientais por fármacos, pesticidas, surfactantes e seus produtos de degradação, dentre outros. No presente trabalho, foram propostos dois métodos para estudar as águas oriundas do esgoto anterior e posterior ao tratamento ocorrido na ETE do município de São Carlos-SP: análises de compostos orgânicos não específicos por meio da espectroscopia de RMN 1D (1H e 13C) e 2D (COSY, HSQC e HMBC), com o intuito de caracterizar o maior número de substâncias dissolvidas nas matrizes; análises desenvolvidas através do sistema hifenado HPLC-(UV/MS)-SPE-ASS-NMR, para detectar e elucidar os compostos não específicos recalcitrantes, em baixas concentrações e sem o uso de padrões. Ademais, foram empregadas análises quimiométricas e quantitativas (RMNq) no primeiro método (compostos orgânicos não específicos) para, desta forma, monitorar variações sazonais e identificar descargas anômalas no sistema comum de escoamento do esgoto sanitário doméstico. Portanto, em ambas as matrizes de esgoto (não tratado e tratado pela ETE) foram caracterizados 50 compostos orgânicos, em que as concentrações variaram consideravelmente com o tratamento da ETE e de acordo com a sazonalidade da coleta. Também foram verificados uma descarga anormal no sistema comum de esgoto e influências das águas fluviais sobre a composição das águas de esgoto, além de serem completamente elucidados compostos homólogos recalcitrantes pertencentes a classe dos surfactantes LAS (alquilbenzeno sulfonados de cadeia linear) no efluente. As variações sazonais e anormalidade na composição química no esgoto indicaram que o procedimento empregado pode ser especialmente útil para identificar fontes poluidoras e acompanhar a eficiência do tratamento das ETEs para que, desta forma, sejam tomadas ações preventivas a fim de proteger todo sistema de tratamento e equipamentos e, com isso, minimizar os danos causados ao meio ambiente.
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Schwalbe-Herrmann, Miriam [Verfasser], Dieter [Akademischer Betreuer] Leibfritz et Herbert [Akademischer Betreuer] Thiele. « Lipidanalyse von Bioflüssigkeiten durch kombinierte SPE/HPLC-, MS- und NMR-Techniken / Miriam Schwalbe-Herrmann. Gutachter : Dieter Leibfritz ; Herbert Thiele. Betreuer : Dieter Leibfritz ». Bremen : Staats- und Universitätsbibliothek Bremen, 2013. http://d-nb.info/107208306X/34.
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Benešová, Markéta. « Stanovení léčiv pomocí HPLC s různými typy detektorů ». Master's thesis, Vysoké učení technické v Brně. Fakulta chemická, 2011. http://www.nusl.cz/ntk/nusl-216704.
Texte intégralRésumé :
This diploma thesis deals with the determination of macrolide antibiotics in wastewater, especially with erythromycin, clarithromycin and roxithromycin. In this time are these pharmaceuticals prescribed quite frequently. Solid phase extraction (SPE) was used for the isolation and the purification of selected analytes from an aqueous matrix; as the suitable procedure was found the using Oasis HLB cartridges. High performance liquid chromatography with mass spectrometry detection (HPLC-MS) was optimized for its analysis of selected pharmaceuticals. The optimized method was used for the determination of pharmaceuticals in real water samples, which was taken at the inflow and the outflow of the urban wastewater treatment plant in Brno-Modřice.
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Rolisola, Ana Marta Cavinato Marchini [UNESP]. « Análise de especiação e fracionamento de biocidas de zinco (Piritionato de zinco, Zineb e Ziram) utilizando SPE, DGT, HPLC e ICP-MS em água estuarina ». Universidade Estadual Paulista (UNESP), 2018. http://hdl.handle.net/11449/154339.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
Atualmente, cerca de 18 compostos são utilizados como biocidas de reforço (metálicos) em tintas anti-incrustantes, como por exemplo Piritionato de Zinco (Zn(PT)2), Zineb e Ziram. É relevante o desenvolvimento de um método analítico para determinação das concentrações ambientais de biocidas metálicos. O presente estudo teve como objetivos i)desenvolver uma metodologia de extração em fase sólida (SPE) e cromatografia líquida de alta eficiência acoplada (HPLC) ao espectrômetro de massas com plasma acoplado indutivamente (ICP-MS) para determinação de Zn(PT)2, Zineb e Ziram e ii) quantificar, in lab, a fração lábil total do Piritionato de Zinco, Zineb e Ziram e in situ, a fração lábil total do zinco, utilizando a técnica de difusão em filmes finos por gradiente de concentração (DGT) em solução padrão e água estuarina, respectivamente. Na técnica de SPE foi utilizado o sorbente de sílica funcionalizado com fenil apresentando excelente retenção para Zn(PT)2, Zineb e Ziram (94 ± 0,1%, 85 ± 0,04% e 93 ± 0,1%, respectivamente) e recuperações entre 85% e 110%. Na determinação dos biocidas de zinco utilizando o acoplamento HPLC-VGroove-ICP-MS com diluição pós coluna cromatográfica, a fase móvel composta por metanol e 0,006 mol L-1 de acetato de amônio (50:50, v v-1) apresentou o melhor desempenho na separação do Zn(PT)2, Zineb, Ziram. A curva analítica obtida para o Zn(PT)2 apresentou coeficiente de correlação, LD e LQ satisfatórios para os isótopos 64Zn (0,98, 0,575 mg L-1, 1,916 mg L-1), 66Zn(0,99, 0,480 mg L-1 , 1,600 mg L-1), 68Zn(0,98, 0,602 mg L-1, 2,007 mg L-1). Na técnica DGT foi utilizado o agente ligante resina Chelex® 100 para avaliar a labilidade do Zn(PT)2, Zineb e Ziram em água estuarina. Os resultados demonstraram que a fração lábil total do Zn ficou em torno de 100% para o Zineb (111%) e Ziram (109%), ou seja, estes biocidas formaram espécies totalmente lábeis na amostra de água estuarina e para Zn(PT)2 foi de 75% indicando espécies parcialmente lábeis. Os resultados obtidos na técnica SPE, no acoplamento HPLC-VGroove-ICP-MS e DGT demonstraram que os métodos apresentam desempenho satisfatório para a determinação de Piritionato de Zinco, Zineb e Ziram.
About 18 compounds are used as booster biocides (metal) in antifouling paints such as Zinc Pyrithione (Zn(PT)2), Zineb and Ziram. It is important to develop an analytical method for determining of the environmental concentrations of zinc biocides. The present study had as objectives i) to develop a solid phase extraction (SPE) and high performance liquid chromatography (HPLC) coupled to the inductively coupled plasma mass spectrometer (ICP-MS) for the determination of Zn(PT)2, Zineb and Ziram and ii) quantify in lab the total labile fraction of Zn(PT)2, Zineb and Ziram and in situ the total labile fraction of zinc using the diffusive gradient in thin films (DGT) technique in standard solution and estuarine water, respectively. In the SPE technique, the silica sorbent functionalized with phenyl presented excellent retention for Zn(PT)2, Zineb and Ziram (94 ± 0.1%, 85 ± 0.04% and 93 ± 0.1%, respectively) and recoveries between 85% and 110%. In the determination of zinc using the HPLC-VGroove-ICP-MS coupling with post-column chromatographic dilution, the mobile phase composed of methanol and 0.006 mol L-1 of ammonium acetate (50:50, v v-1) of presented the best performance in the separation of Zn(PT)2, Zineb and Ziram. The analytical curve obtained for Zn(PT)2 presented satisfactory correlation coefficient, LD and LQ for the isotopes 64Zn (0.98, 0.575 mg L -1, 1.916 mg L-1), 66Zn (0.99, 0.480 mg L-1, 1.600 mg L-1), 68Zn (0.98, 0.602 mg L-1, 2.007 mg L-1). In the DGT technique, the Chelex® 100 resin binder was used to evaluate the lability of the zinc biocides Zn(PT)2, Zineb and Ziram in estuarine water. The results showed that the total labile fraction of Zn was around 100% for Zineb (111%) and Ziram (109%), that is, these biocides formed totally labile species in the estuarine water sample and for Zn(PT)2 was 75% indicating partially labile species. The results obtained in the SPE technique in the HPLC-VGroove-ICP-MS coupling and DGT demonstrated that the methods present satisfactory performance for the determination of Zn(PT)2, Zineb and Ziram.
CNPq: 164326/2015.
FAPESP: 2015/03397-4.
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Rolisola, Ana Marta Cavinato Marchini. « Análise de especiação e fracionamento de biocidas de zinco (Piritionato de zinco, Zineb e Ziram) utilizando SPE, DGT, HPLC e ICP-MS em água estuarina / ». Rio Claro, 2018. http://hdl.handle.net/11449/154339.
Texte intégralRésumé :
Orientador: Amauri Antonio MenegárioBanca: Didier Gastmans
Banca: Lauren Nozomi Marques Yabuki
Banca: Luciana Polese
Banca: Anne Hélène Fostier
Resumo: Atualmente, cerca de 18 compostos são utilizados como biocidas de reforço (metálicos) em tintas anti-incrustantes, como por exemplo Piritionato de Zinco (Zn(PT)2), Zineb e Ziram. É relevante o desenvolvimento de um método analítico para determinação das concentrações ambientais de biocidas metálicos. O presente estudo teve como objetivos i)desenvolver uma metodologia de extração em fase sólida (SPE) e cromatografia líquida de alta eficiência acoplada (HPLC) ao espectrômetro de massas com plasma acoplado indutivamente (ICP-MS) para determinação de Zn(PT)2, Zineb e Ziram e ii) quantificar, in lab, a fração lábil total do Piritionato de Zinco, Zineb e Ziram e in situ, a fração lábil total do zinco, utilizando a técnica de difusão em filmes finos por gradiente de concentração (DGT) em solução padrão e água estuarina, respectivamente. Na técnica de SPE foi utilizado o sorbente de sílica funcionalizado com fenil apresentando excelente retenção para Zn(PT)2, Zineb e Ziram (94 ± 0,1%, 85 ± 0,04% e 93 ± 0,1%, respectivamente) e recuperações entre 85% e 110%. Na determinação dos biocidas de zinco utilizando o acoplamento HPLC-VGroove-ICP-MS com diluição pós coluna cromatográfica, a fase móvel composta por metanol e 0,006 mol L-1 de acetato de amônio (50:50, v v-1) apresentou o melhor desempenho na separação do Zn(PT)2, Zineb, Ziram. A curva analítica obtida para o Zn(PT)2 apresentou coeficiente de correlação, LD e LQ satisfatórios para os isótopos 64Zn (0,98, 0,575 mg L-1, 1,916 mg L-1... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: About 18 compounds are used as booster biocides (metal) in antifouling paints such as Zinc Pyrithione (Zn(PT)2), Zineb and Ziram. It is important to develop an analytical method for determining of the environmental concentrations of zinc biocides. The present study had as objectives i) to develop a solid phase extraction (SPE) and high performance liquid chromatography (HPLC) coupled to the inductively coupled plasma mass spectrometer (ICP-MS) for the determination of Zn(PT)2, Zineb and Ziram and ii) quantify in lab the total labile fraction of Zn(PT)2, Zineb and Ziram and in situ the total labile fraction of zinc using the diffusive gradient in thin films (DGT) technique in standard solution and estuarine water, respectively. In the SPE technique, the silica sorbent functionalized with phenyl presented excellent retention for Zn(PT)2, Zineb and Ziram (94 ± 0.1%, 85 ± 0.04% and 93 ± 0.1%, respectively) and recoveries between 85% and 110%. In the determination of zinc using the HPLC-VGroove-ICP-MS coupling with post-column chromatographic dilution, the mobile phase composed of methanol and 0.006 mol L-1 of ammonium acetate (50:50, v v-1) of presented the best performance in the separation of Zn(PT)2, Zineb and Ziram. The analytical curve obtained for Zn(PT)2 presented satisfactory correlation coefficient, LD and LQ for the isotopes 64Zn (0.98, 0.575 mg L -1, 1.916 mg L-1), 66Zn (0.99, 0.480 mg L-1, 1.600 mg L-1), 68Zn (0.98, 0.602 mg L-1, 2.007 mg L-1). In the DGT technique, t... (Complete abstract click electronic access below)
Doutor
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Bettioui, Terkia. « Lipidomique du globule rouge par des techniques de spectrométrie de masse et d'imagerie infrarouge : Application à l'étude de la maladie de Gaucher ». Electronic Thesis or Diss., université Paris-Saclay, 2024. http://www.theses.fr/2024UPASF085.
Texte intégralRésumé :
Les globules rouges suscitent un intéret clinique particulier en raison de leur importance biologique. Il a été récemment démontré que certaines pathologies érythrocytaires pouvaient être associées à une composition lipidique anormale. Parmi ces pathologies figure la maladie de Gaucher, un trouble lysosomal rare causé par une déficience en β-glucocérébrosidase, enzyme dont l'absence entraîne une accumulation excessive de certains sphingolipides dans l'organisme. Cette surcharge lipidique altère les propriétés morphologiques et rhéologiques des globules rouges, provoquant des anomalies hématologiques et vasculaires.Dans cette thèse, nous avons étudié le lien entre la composition lipidique des globules rouges et son implication dans la maladie de Gaucher. En particulier, nous nous sommes concentrés sur deux catégories de lipides : les sphingolipides et les phospholipides, qui jouent un rôle clé dans les altérations érythrocytaires observées. Deux approches complémentaires ont été utilisées : la première utilise la spectrométrie de masse dans le but d'identifier de nouveaux biomarqueurs. La seconde exploite des techniques d'imagerie infrarouge à différentes échelles pour étudier la répartition des lipides dans les globules rouges.Nous avons mis au point une méthode rapide de préparation d'échantillons en ligne avec la chromatographie liquide couplée à la spectrométrie de masse (SPE-HPLC-MS/MS), pour doser 30 sphingolipides et phospholipides en moins de 15 min. Par la suite cette méthode a été appliquée pour quantifier les 30 espèces lipidiques dans le plasma et le culot globulaire de sujets contrôles et de patients Gaucher. Parmi ces espèces lipidiques, certaines étaient surexprimées et n'étaient pas associées à la maladie de Gaucher, ouvrant de nouvelles perspectives pour le diagnostic et le suivi thérapeutique.A l'issue de ce dosage nous nous sommes intéressés à l'exploration du lipidome du globule rouge sain pour pouvoir le comparer à celui du globule rouge Gaucher. Pour cela une approche semi-ciblée a été menée en utilisant un analyseur triple quadripolaire. Ceci nous a permis d'identifier plus de 266 espèces moléculaires réparties sur 12 classes lipidiques différentes.Ces résultats ont contribué à une meilleure connaissance du lipidome du globule rouge sain et sont prometteurs pour l'identification de nouveaux biomarqueurs et la compréhension de diverses pathologies affectant le lipidome érythrocytaire.En complément de cette approche, nous avons étudié la morphologie et la composition chimique des globules rouges en utilisant des techniques d'imagerie vibrationnelle infrarouge à différentes résolutions : à l'échelle microscopique avec la microspectroscopie infrarouge à transformée de Fourier (μ-FTIR), à l'échelle submicronique avec l'imagerie optique thermique (O-PTIR) et à l'échelle nanométrique grâce à l'AFM-IR.Cette étude a été réalisée en trois étapes principales : (1) l'élaboration d'un protocole de préparation permettant la fixation des globules rouges, (2) l'évaluation de leur stabilité chimique et morphologique, et enfin (3) une analyse multi-échelles comparant des globules rouges sains à ceux affectés par la maladie de Gaucher.Grâce à notre protocole de fixation, nous avons pu préserver les globules rouges sans altération pendant 10 jours, ce qui nous a permis de mener à bien l'analyse multi-échelle. L'AFM-IR s'est révélée être la seule technique capable de mettre en évidence des différences significatives entre les globules rouges sains et Gaucher. L'AFM-IR a permis de visualiser les différentes morphologies des cellules Gaucher et de comparer la distribution des lipides à travers des cartographies chimiques, révélant des zones d'intérêt au niveau de la membrane érythrocytaireRed blood cells attract particular clinical interest due to their biological significance. It has recently been demonstrated that certain erythrocyte pathologies may be associated with abnormal lipid composition. Among these pathologies is Gaucher's disease, a rare lysosomal disorder caused by a deficiency in β-glucocerebrosidase, an enzyme whose absence leads to excessive accumulation of certain sphingolipids in the body. This lipid overload alters the morphological and rheological properties of red blood cells, causing hematological and vascular abnormalities.In this thesis, we studied the link between the lipid composition of red blood cells and its implication in Gaucher's disease. In particular, we focused on two categories of lipids: sphingolipids and phospholipids, which play a key role in the erythrocyte alterations observed. Two complementary approaches were used: the first uses mass spectrometry with the aim of identifying new biomarkers. The second uses infrared imaging techniques at different scales to study the distribution of lipids in red blood cells.We developed a rapid sample preparation method compatible with liquid chromatography coupled to mass spectrometry (SPE-HPLC-MS/MS) to quantify 30 sphingolipids and phospholipids in less than 15 minutes. This method was then applied to quantify the 30 lipid species in the plasma and red blood cell pellet of control subjects and Gaucher patients Among these lipid species, some were overexpressed and were not associatedAfter this quantification, we focused on exploring the lipidome of healthy red blood cells and comparing it to that of Gaucher red blood cells. To achieve this, a semi-targeted approach was conducted using a triple-quadrupole analyzer, which allowed us to identify more than 266 molecular species spread across 12 different lipid classes.These results have contributed to a better understanding of the lipidome of healthy red blood cells and are promising for the identification of new biomarkers and the diagnosis of various pathologies affecting the erythrocyte lipidome.As a complement to this approach, we focused on the morphological and chemical study of red blood cells using vibrational infrared imaging techniques at different resolutions: microscopic with Fourier-transform infrared spectroscopy (FTIR), submicron with optical photothermal infrared imaging (O-PTIR), and nanometric with atomic force microscopy (AFM-IR).Our study was structured around three steps: (1) developing a preparation protocol allowing the fixation of red blood cells, (2) evaluating their chemical and morphological stability, and finally (3) conducting a multi-scale analysis comparing healthy red blood cells with those affected by Gaucher's disease.Due to our fixation protocol, we were able to preserve red blood cells without degradation for 10 days, which enabled us to successfully conduct the multi-scale analysis. AFM-IR proved to be the only technique capable of highlighting significant differences between healthy and Gaucher red blood cells. AFM-IR allowed us to visualize the distinct morphologies of Gaucher cells and to compare lipid distribution through chemical mapping, revealing areas of interesting in the erythrocyte membrane
Actes de conférences sur le sujet "SPE-HPLC-MS/MS"
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Sun, Jing, Xi-Kui Wang, Ru-Yi Xu, Xia Wang et Ru-Song Zhao. « Notice of Retraction : Sensitive Determination of Triclosan in Water Using SPE Packed with Bamboo Carbon Combined with HPLC-ESI-MS ». Dans 2011 5th International Conference on Bioinformatics and Biomedical Engineering. IEEE, 2011. http://dx.doi.org/10.1109/icbbe.2011.5780744.
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Weissenberger, Markus Christian, et Sukhmeet Dhillon. « Interrelationship of Weak Organic Acids, Bases, pH and HPLC Analysis Method in Produced Waters ». Dans SPE/CSUR Unconventional Resources Conference – Canada. Society of Petroleum Engineers, 2014. http://dx.doi.org/10.2118/171650-ms.
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Tumewu, Putranda Yeremia, et Ester Tio Minar E. Silalahi. « Chemical Tracer Application to Compare Napthalene Sulfonic Acid and Sodium Fluorobenzoic Acid as Part of Polymer Field Trial Project ». Dans SPE Improved Oil Recovery Conference. SPE, 2024. http://dx.doi.org/10.2118/218180-ms.
Texte intégralRésumé :
Abstract Tracer testing is the effective method to characterize subsurface, especially to investigate well connectivity or fluid pathways, estimate traveling velocity of injected fluid, assess the breakthrough times of the tracers between injectors and producers, and evaluate swept pore volume and sweep efficiency particularly in Enhanced Oil Recovery (EOR) operation. Fluoro-benzoic acid (FBA) remains the primary and most common liquid phase tracer in oil industry, but recent laboratory and geothermal field test using Naphthalene Sulfonic Acid (NSA) also looks very promising. The NSAs are thermally stable at reservoir conditions, cost about a tenth of the cost of FBAs, and have a much lower detection limit when tested using High Performance Liquid Chromatograph (HPLC). The drawback is that they have not been widely tested in oil reservoir but have proven themselves in the laboratory tests and in geothermal reservoirs. This paper describes performance test of NSA as chemical tracer in oil reservoir in direct comparison with proven conservative tracer, FBA by pairing an NSA tracer with a proven FBA tracer in the same injector well as part of IOR polymer pilot project. Six different types of NSAs were injected at the six different injection wells. In addition, six different types of FBAs were also injected at the same wells to make comparative data with NSA at producer wells. The tracer test was performed for 170 days with relatively constant injection and producing rate to maintain steady state condition in the reservoir. The injection and production rates were balanced for the test duration. Bottom-hole temperature is about 85°C.
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Liu, Ya, Dong Lee, Haiping Lu et Jeffrey Russek. « Development of Fluorescence Tagged Scale Inhibitors for Squeeze Applications in Gulf of Mexico ». Dans SPE International Conference on Oilfield Chemistry. SPE, 2021. http://dx.doi.org/10.2118/204349-ms.
Texte intégralRésumé :
Abstract Fluorescence tagged (F-tagged) scale inhibitors are drawing more interest in the oil industry and are being applied in the field. One main reason is being easily detectable and differentiable from other scale inhibitors. However, when applied to a new oilfield, it is necessary to evaluate their thermal stability, limit of detection (LOD), and fluorescence measurement interference from other chemicals. Two F-tagged scale inhibitors were tested in this study. They are the same polymeric inhibitors with different and differentiable fluorescent tags. Both F-tagged inhibitors were able to be detected in synthetic brine and field brine from a Gulf of Mexico (GoM) field, with LOD of 1ppm. A coreflood test was also conducted for inhibitor squeeze treatment evaluation. The residual scale inhibitor in core flooding samples was measured by both fluorescence method and high performance liquid chromatography (HPLC). The results from two methods generally match with each other. This strongly indicates that the F-tag is stable on scale inhibitors and fluorescence measurement is a reliable method for scale inhibitor detection. Thermal aging test and long storage test were conducted. For both F-tagged scale inhibitors, the thermal aged samples and samples with different storage lifetime did not show significant difference on scale inhibition performance and fluorescence measurement. The two F-tagged inhibitors tested can tolerate high temperature up to at least 130°C (266°F). With proper storage, F-tagged inhibitors after long shelf storage were still as effective as fresh inhibitors. Based on all the test results in this paper, these two scale inhibitors are ready for squeeze application in GoM.
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Ow, Hooisweng, Sehoon Chang, Gawain Thomas, Wei Wang, Afnan A. Mashat et Hussein Shateeb. « Automatable High Sensitivity Tracer Detection : Toward Tracer Data Enriched Production Management of Hydrocarbon Reservoirs ». Dans SPE Annual Technical Conference and Exhibition. SPE, 2021. http://dx.doi.org/10.2118/206338-ms.
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Abstract The development of automatable high sensitivity analytical methods for tracer detection has been one of the most central challenges to realize ubiquitous full-field tracer deployment to study reservoirs with many cross-communicating injector and producer wells. Herein we report a tracer analysis approach, inspired by strategies commonly utilized in the biotechnology industry, that directly addresses key limitations in process throughput, detection sensitivity and automation potential of state-of-the-art technologies. A two-dimensional high performance liquid chromatography (2D-HPLC) method was developed for the rapid fluorescence detection and simultaneous identification of a class of novel barcoded tracers in produced water down to ultra-trace concentration ranges (<1ppb), matching the sensitivity of tracer technologies currently used in the oil industry. The sample preparation process throughput was significantly intensified by judicious adaptations of off-the-shelf biopharma automation solutions. The optical detection sensitivity was further improved by the time-resolved luminescence of the novel tracer materials that allows the negation of residual background signals from the produced water. To showcase the potential, we applied this powerful separation and detection methodology to analyze field samples from two recent field validations of a novel class of optically detectable tracers, in which two novel tracers were injected along with a benchmarking conventional fluorobenzoic acid (FBA)-based tracer. The enhanced resolving power of the 2D chromatographic separation drastically suppressed the background signal, enabling the optical detection of a tracer species injected at 10x lower concentration. Further, we orthogonally confirmed the detection of this tracer species by the industry standard high-resolution accurate mass spectrometry (HRAM) technique, demonstrating comparable limits of detection. Tracer detection profile indicated that the transport behavior of the novel optical tracers through highly saline and retentive reservoir was similar to that of FBAs, validating the performance of this new class of tracers. Promising steps toward complete automation of the tracer separation and detection procedure have drastically reduced manual interventions and decreased the analysis cycle time, laying solid foundation to full-field deployment of tracers for better reservoir characterizations to inform decisions on production optimization. This paper outlines the automatable tracer detection methodology that has been developed for robustness and simplicity, so that efficient utilization of the resultant high-resolution tracer data can be applied toward improving production strategy via intelligent and active rate adjustments.
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Taylor, Grahame, Jonathan Wylde et Bridgette Allan. « Novel H2S Scavenger Testing Methodology to Meet the Ever-Present Challenge of Simulating Scavenger Application Methods with Laboratory Testing Protocols ». Dans SPE International Conference on Oilfield Chemistry. SPE, 2021. http://dx.doi.org/10.2118/204356-ms.
Texte intégralRésumé :
Abstract The design methodology for H2S scavengers relies heavily on developing a test protocol that most closely simulates field applications. These include gas contact towers, direct gas production injection and multiphase treatments, such as subsea umbilical delivery lines to sea floor well heads, hydrocarbon flow lines and sour storage tank treatments. There are very few testing standards and while there are industry accepted methods, the novel methods presented fill the gaps that exist. A thorough review is made of existing test methodologies such as the static gas breakthrough test and the multiphase Parr Autoclave. Each of these has become an accepted, albeit unofficial, industry standard. Novel methods recently developed comprise the "Direct Injection Laboratory Simulator" (DILS) which, as the name suggests, represents a laboratory method of evaluating a direct gas injection application. Also included is a unique modification of the gas breakthrough test, known as the "miniature Ultrafab tower" which simulates a regenerative tower-based system, commonly in operation in the field. The results showed fascinating validation of gas direct injection and dynamic tower interactions. In some cases, the results are as expected and in others fresh insight has been obtained into any observed discrepancy between a scavenger's field performance and how it performs in the laboratory development studies. In the case of the "miniature Ultrafab tower", this ingenious piece of equipment has been proven to accurately simulate the packing typically seen in the gas contactor to enhance gas/liquid interaction as well as provides the ability to continually replenish the tower with fresh chemical during the test using an accurately controlled flow rate from an HPLC pump. These have been shown to be vitally important parameters for accurate lab to field correlation and are uniquely available from this test, for example gleaning the minimum flow rate of fresh scavenger which can control the H2S concentration to the predetermined level; exactly as is done in field operations. This novel apparatus also has a separator chamber where the spent chemical can be collected, analyzed and evaluated, exactly as is done in a field trial for a dynamic contact gas tower. Armed with a new series of test methodologies, the development of H2S scavengers can enjoy a much higher success rate in the all-important transition from laboratory to field. The test methods also give invaluable tools to trouble shooting and investigate unexpected deficiencies in products which have in the past performed as expected. This includes providing a validation method for changes and enhancements desired during the manufacture process and raw material sourcing for chemical scavengers.
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Chen, Hsieh, Sehoon Chang, Gawain Thomas, Wei Wang, Afnan Mashat et Hussain Shateeb. « Comparison of Water and Gas Tracers Field Breakthrough ». Dans SPE Annual Technical Conference and Exhibition. SPE, 2021. http://dx.doi.org/10.2118/205863-ms.
Texte intégralRésumé :
Abstract We are developing new classes of barcoded advanced tracers, which, compared to present commercial offerings, can be optically detected in an automated fashion. The eventual goal for the advanced tracers is to deploy cost-effective, ubiquitous, long-term, and full-field tracer tests in supporting large-scale waterflooding optimization for improved oil recovery. In this paper, we compare model predictions to breakthrough data from two field tests of advanced tracers in a pilot during water alternating gas (WAG) cycles, where gas tracer tests have recently been performed as well. Two advanced tracer injections were performed at the test site. For the first injection, only a dipicolinic acid based advanced tracer (DPA) was injected. For the second injection, DPA and a phenanthroline- based advanced tracer, 4,7-bis(sulfonatophenyl)-1,10-phenanthroline-2,9-dicarboxylic acid (BSPPDA), was injected in conjunction with a commercially available fluorobenzoic acid-based tracer (FBA) to benchmark their performance. Produced water samples were collected weekly for tracer analysis. Both newly developed 2D-high performance liquid chromatography/time-resolved fluorescence optical detection method (2D-HPLC/TRF) and liquid chromatography-mass spectrometry (LC-MS) were used to construct the breakthrough curves for the advanced tracers. In parallel, gas chromatography-mass spectrometry (GC-MS) was used to detect FBA tracer. Gas tracer tests have been performed on the same field. Since DPA, BSPPDA and FBA tracers were water tracers as designed, they were expected to appear in between gas tracer breakthroughs, and we observed exactly that for BSPPDA and FBA. Unexpectedly, the DPA predominantly appeared along with gas tracer breakthroughs, suggesting its favorable compatibility with the gas phase. We suspect the presence of some gas components rendered the medium more acidic, which likely protonates DPA molecules, thereby alters its hydrophilicity. A wealth of information could be gathered from the field tests. First, all tracers survived not only the harsh reservoir conditions but also the irregular WAG injections. Their successful detection from the producers suggested robustness of these materials for reservoir applications. Second, the breakthrough curves of the BSPPDA tracers using optical detection method were very similar to those of FBA tracers detected by GC-MS, substantiating the competency of our in-house materials and detection methods to the present commercial offerings. Finally, even though DPA has passed prior lab tests as a good water tracer, its high solubility to gas phase warrants further investigation. This paper summarizes key results from two field trials of the novel barcoded advanced tracers, of which both the tracer materials and detection methods are new to the industry. Importantly, the two co- injected advanced tracers showed opposite correlations to the gas tracers, highlighting the complex physicochemical interactions in reservoir conditions. Nevertheless, the information collected from the field trials is invaluable in enabling further design and utilization of the advanced tracers in fulfilling their wonderful promises.
Rapports d'organisations sur le sujet "SPE-HPLC-MS/MS"
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Crouch, Rebecca, Jared Smith, Bobbi Stromer, Christian Hubley, Samuel Beal, Guilherme Lotufo, Afrachanna Butler et al. Preparative, extraction, and analytical methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil or sediment, and tissue matrices. Engineer Research and Development Center (U.S.), août 2021. http://dx.doi.org/10.21079/11681/41480.
Texte intégralRésumé :
No standard method exists for determining levels of insensitive munition (IM) compounds in environmental matrices. This project resulted in new methods of extraction, analytical separation and quantitation of 17 legacy and 7 IM compounds, daughter products of IM, and other munition compounds absent from USEPA Method 8330B. Extraction methods were developed for aqueous (direct-injection and solid-phase extraction [SPE]), soil, sediment, and tissue samples using laboratory-spiked samples. Aqueous methods were tested on 5 water sources, with 23 of 24 compounds recovered within DoD QSM Ver5.2 limits. New solvent extraction (SE) methods enabled recovery of all 24 compounds from 6 soils within QSM limits, and a majority of the 24 compounds were recovered at acceptable levels from 4 tissues types. A modified chromatographic treatment method removed analytical interferences from tissue extracts. Two orthogonal high-performance liquid chromatography-ultraviolet (HPLC-UV) separation methods, along with an HPLC–mass spectrometric (HPLC-MS) method, were developed. Implementing these new methods should reduce labor and supply costs by approximately 50%, requiring a single extraction and sample preparation, and 2 analyses rather than 4. These new methods will support environmental monitoring of IM and facilitate execution of risk-related studies to determine long-term effects of IM compounds.
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Crouch, Rebecca, Jared Smith, Bobbi Stromer, Christian Hubley, Samuel Beal, Guilherme Lotufo, Afrachanna Butler et al. Methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil/sediment, and tissue matrices. Engineer Research and Development Center (U.S.), août 2021. http://dx.doi.org/10.21079/11681/41720.
Texte intégralRésumé :
Currently, no standard method exists for analyzing insensitive munition (IM) compounds in environmental matrices, with or without concurrent legacy munition compounds, resulting in potentially inaccurate determinations. The primary objective of this work was to develop new methods of extraction, pre-concentration, and analytical separation/quantitation of 17 legacy munition compounds along with several additional IM compounds, IM breakdown products, and other munition compounds that are not currently included in U.S. Environmental Protection Agency (EPA) Method 8330B. Analytical methods were developed to enable sensitive, simultaneous detection and quantitation of the 24 IM and legacy compounds, including two orthogonal high-performance liquid chromatography (HPLC) column separations with either ultraviolet (UV) or mass spectrometric (MS) detection. Procedures were developed for simultaneous extraction of all 24 analytes and two surrogates (1,2-dinitrobenzene, 1,2-DNB; o-NBA) from high- and low-level aqueous matrices and solid matrices, using acidification, solid phase extraction (SPE), or solvent extraction (SE), respectively. The majority of compounds were recovered from four tissue types within current limits for solids, with generally low recovery only for Tetryl (from 4 to 62%). A preparatory chromatographic interference removal procedure was adapted for tissue extracts, as various analytical interferences were observed for all studied tissue types.