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A new facile, rapid, inexpensive, and sensitive method for the analysis of six trace trichlorophenols in seawater samples was developed by magnetic micro-solid-phase extraction coupled to liquid chromatography with tandem mass spectrometry. Core-shell covalently functionalized ferroferric oxide coated with aminated silicon dioxide and decorated with multiwalled carbon nanotubes was applied as an adsorbent to perform the extraction process. The effect of factors including solution pH, contact time, adsorbent amount, and ionic strength were investigated in detail. The obtained results revealed that the proposed adsorbent was a highly effective and low-cost magnetic micro-solid-phase extraction material for the enrichment of 2,3,4-trichlorophenol, 2,3,5-trichlorophenol, 2,3,6-trichlorophenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, and 3,4,5-trichlorophenol from seawater. Under the optimized conditions, the recoveries ranged from 88.0 to 99.5% at the three spiking levels, the limits of detection and the limits of quantification were 0.002 and 0.007 µg/L for the six trichlorophenols, respectively. The intra- and interday relative standard deviations were 2.0-6.7 and 4.5-8.9%, respectively. The calibration curves showed a good linearity in the range of 0.02-5.0 µg/L. The routine run analyses showed that the developed method was fast, simple, accurate, solvent-saving and high resolution, and it was suitable for the determination of trace trichlorophenols in seawater.
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A novel triethylenetetramine-functionalized magnetic graphene oxide composite was prepared and used as a magnetic solid-phase extraction adsorbent for the fast detection of ten trace-level phenolic environmental estrogens in environmental water. The synthesized material was carefully characterized by scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometry, and X-ray photoelectron spectroscopy to confirm the structure and components. The adsorption and desorption conditions of the adsorbent toward phenolic environmental estrogens were optimized in detailed to obtain the best extraction recovery and elution efficiency. Under the optimum conditions, the limits of detection of the method for ten phenolic environmental estrogens were in range of 0.15-1.5 ng/L, which was lower than the reported methods for phenolic environmental estrogens detection in literatures. This could be contributed to the unique structure and property of the as-prepared material. The developed method was successfully applied for the determination of environmental water samples with recoveries ranging from 88.5 to 105.6%.
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Estrógenos/química , Grafito/química , Magnetismo , Óxidos/química , Fenol/química , Trientina/química , Agua/química , Adsorción , Cromatografía Líquida de Alta Presión , Monitoreo del Ambiente/métodos , Contaminantes Ambientales , Límite de Detección , Impresión Molecular , Polímeros/química , Reproducibilidad de los Resultados , Solventes/química , Contaminantes Químicos del Agua/químicaRESUMEN
[This corrects the article DOI: 10.1039/C4RA14150D.].
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This article has been retracted at the request of the Editor after the corresponding author pointed the Editor to comments from an anonymous reader. The article reports electron micrographs of different preparations while showing identical images as used in previous publications by the same authors. The particles in Fig. 4C (SEM image of Fe3O4@SiO2) are identical to each other and the corresponding author confirmed that these have been copy-pasted. In addition, these particles have previously been communicated as different substances in Fig. 1B from Pan et al., J. Mater. Chem. A, 2015,3, 23042-23052 (DOI: 10.1039/C5TA05840F) and Fig. 3F from Pan et al., Anal. Methods, 2017,9, 5281-5292 (DOI: 10.1039/C7AY01444A). Furthermore, the curves in Fig. 7, especially the baseline, shows a remarkable similarity to Fig. 8 from Pan et al., J. Mater. Chem. A, 2015,3, 23042-23052 (DOI: 10.1039/C5TA05840F) and Fig. 5F from Pan et al., J. Mater. Chem. A, 2014,2, 15345-15356 (DOI: 10.1039/c4ta02600d). The manipulation of images and data in this way is a serious offense to the integrity of the scientific community and casts doubts on all the data, and accordingly also the conclusions based on that data, in this publication. As such this article represents a severe abuse of the scientific publishing system. The scientific community takes a very strong view on this matter and apologies are offered to readers of the journal that this was not detected during the submission process. This article has been retracted: please see Elsevier Policy on Article Withdrawal (https://www.elsevier.com/about/our-business/policies/article-withdrawal).
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An effective method has been developed for the simultaneous determination of four bisphenols (bisphenol A, S, F and B) in various foodstuffs. The contaminants were extracted by QuEChERS-based strategy and subjected to ion-exchange solid-phase extraction for further clean-up. The critical variables were screened by Plackett-Burman design and then optimized by central composite design. Under the optimized conditions, satisfactory accuracy (recoveries 76%-116%) and precision (RSDsâ¯<â¯12%) were achieved. The established method was then used to assess the contamination status of 379 real samples. Bisphenol A was demonstrated to be the predominant bisphenol with highest incidence (79.7%) and average concentration (14.3⯵g/kg). The positive rates (mean concentration) of bisphenol S, F and B were 37.7% (1.6⯵g/kg), 26.9% (1.4⯵g/kg) and 0.0% (not detected), respectively. Finally, the daily dietary intakes of ∑4bisphenolsfor adult residents were estimated (55.9-76.1â¯ng/kgâ¯bw/day) according to the contamination concentrations and the daily recommended intakes.
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Compuestos de Bencidrilo/análisis , Análisis de los Alimentos/métodos , Fenoles/análisis , Sulfonas/análisis , Compuestos de Bencidrilo/aislamiento & purificación , Cromatografía Líquida de Alta Presión , Exposición Dietética , Humanos , Límite de Detección , Fenoles/aislamiento & purificación , Extracción en Fase Sólida , Sulfonas/aislamiento & purificación , Espectrometría de Masas en TándemRESUMEN
Bimetallic oxide CuFeO2 as a new heterogeneous catalyst has shown much higher catalytic ability for activating peroxide than single-metal oxides. The present work demonstrated a synergistic microwave (MW) enhanced Fenton-like process with CuFeO2 for rapid decolorization of azo dye Orange G (OG). The MW irradiation dramatically enhanced the OG degradation efficiency, achieving 99.9% decolorization within 15min at pH5. The XRD analysis of reused CuFeO2, together with metal leaching tests, indicated merits of recycling for CuFeO2. The subsequent surface element analysis by XPS for fresh and used CuFeO2 showed a complex network for reactions between copper-iron redox pairs and surface hydroxyl groups, leading to a synergistic Fenton-like system accelerated by MW irradiation. In the CuFeO2 initiated Fenton-like reactions, several oxidant species (i.e., OH, O2-, electron hole, and FeIVO) responsible to the OG oxidation were identified by quenching experiments, showing the MW generated high temperature and "hot spots" enhanced the yield of OH by generation of electron-hole pairs. Further, the 26 detected degradation products confirmed the OH dominant oxidation of OG. This study shows that the MW-enhanced Fenton-like reaction using CuFeO2 has potential applications for rapid decolorization of dye effluent.
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BACKGROUND: Weight-based dosing strategy is still challenging due to poor awareness and adherence. It is necessary to let clinicians know of the latest developments in this respect and the correct circumstances in which weight-based dosing is of clinical relevance. METHODS: A literature search was conducted using PubMed. RESULTS: Clinical indications, physiological factors, and types of medication may determine the applicability of weight-based dosing. In some cases, the weight effect may be minimal or the proper dosage can only be determined when weight is combined with other factors. Medications within similar therapeutic or structural class (eg, anticoagulants, antitumor necrosis factor medications, P2Y12-receptor antagonists, and anti-epidermal growth factor receptor antibodies) may exhibit differences in requirements on weight-based dosing. In some cases, weight-based dosing is superior to currently recommended fixed-dose regimen in adult patients (eg, hydrocortisone, vancomycin, linezolid, and aprotinin). On the contrary, fixed dosing is noninferior to or even better than currently recommended weight-based regimen in adult patients in some cases (eg, cyclosporine microemulsion, recombinant activated Factor VII, and epoetin α). Ideal body-weight-based dosing may be superior to the currently recommended total body-weight-based regimen (eg, atracurium and rocuronium). For dosing in pediatrics, whether weight-based dosing is better than body surface-area-based dosing is dependent on the particular medication (eg, methotrexate, prednisone, prednisolone, zidovudine, didanosine, growth hormone, and 13-cis-retinoic acid). Age-based dosing strategy is better than weight-based dosing in some cases (eg, intravenous busulfan and dalteparin). Dosing guided by pharmacogenetic testing did not show pharmacoeconomic advantage over weight-adjusted dosing of 6-mercaptopurine. The common viewpoint (ie, pediatric patients should be dosed on the basis of body weight) is not always correct. Effective weight-based dosing interventions include standardization of weight estimation, documentation and dosing determination, dosing chart, dosing protocol, order set, pharmacist participation, technological information, and educational measures. CONCLUSION: Although dosing methods are specified in prescribing information for each drug and there are no principal pros and cons to be elaborated, this review of weight-based dosing strategy will enrich the knowledge of medication administration from the perspectives of safety, efficacy, and pharmacoeconomics, and will also provide research opportunities in clinical practice. Clinicians should be familiar with dosage and administration of the medication to be prescribed as well as the latest developments.
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The easiness-to-handle of the magnetic dispersive solid phase extraction (Mag-dSPE) procedure was developed for preconcentration of 24 steroid hormones in river water. Ethylenediamine-functionalized magnetic carbon nanotubes (EDA@Mag-CNTs) were synthesised by a simple one-pot reaction and were used as sorbent in Mag-dSPE procedure. The properties of the EDA@Mag-CNTs were characterized by transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). An ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method for determination of 24 steroid hormones in river water at nanograms per liter had been developed with pretreatment of the samples by Mag-dSPE. The obtained results demonstrated the higher extraction capacity of EDA@Mag-CNT Mag-dSPE with recoveries between 82.1 and 113%. The limits of quantification (LOQs) for the steroid hormone were between 0.020 and 1.00 ng/L. The developed method had been successfully applied to 60 river water samples, and it was confirmed that EDA@Mag-CNT Mag-dSPE was a highly effective extraction method for the steroid hormone analyses.
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Hormonas Esteroides Gonadales/análisis , Ríos/química , Extracción en Fase Sólida/métodos , Esteroides/análisis , Espectrometría de Masas en Tándem/métodos , Cromatografía Liquida/métodos , Etilenodiaminas , Nanotubos de Carbono/químicaRESUMEN
Safe medication management and use of high-alert narcotics should arouse concern. Risk management experiences in this respect in a large-scale Joint Commission International (JCI)-accredited academic medical center hospital in the People's Republic of China during 2011-2015, focusing on organizational, educational, motivational, and information technological measures in storage, prescribing, preparing, dispensing, administration, and monitoring of medication are summarized. The intensity of use of meperidine in hospitalized patients in 2015 was one-fourth that in 2011. A 100% implementation rate of standard storage of narcotics has been achieved in the hospital since December 2012. A "Plan, Do, Check, Act" cycle was efficient because the ratio of number of inappropriate narcotics prescriptions to total number of narcotics prescriptions for inpatients decreased from August 2014 to December 2014 (28.22% versus 2.96%, P=0.0000), and it was controlled below 6% from then on. During the journey to good pain management ward accreditation by the Ministry of Health, People's Republic of China, (April 2012-October 2012), the medical oncology ward successfully demonstrated an increase in the pain screening rate at admission from 43.5% to 100%, cancer pain control rate from 85% to 96%, and degree of satisfaction toward pain nursing from 95.4% to 100% (all P-values <0.05). Oral morphine equivalent dosage in the good pain management ward increased from 2.3 mg/patient before June 2012 to 54.74 mg/patient in 2014. From 2011 to 2015, the oral morphine equivalent dose per discharged patient increased from 8.52 mg/person to 20.36 mg/person. A 100% implementation rate of independent double-check prior to narcotics dosing has been achieved since January 2013. From 2014 to 2015, the ratio of number of narcotics-related medication errors to number of discharged patients significantly decreased (6.95% versus 0.99%, P=0.0000). Taken together, continuous quality improvements have been achieved in safe medication management and use of narcotics by an integrated multidisciplinary collaboration during the journey to JCI accreditation and in the post-JCI accreditation era.
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In this study, graphene oxide-encapsulated core-shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach between positive charged poly(diallyldimethylammonium) chloride (PDDA)-modified Fe3O4@SiO2 and negative charged GO sheets via electrostatic interaction. The as-prepared GOE-CS-MM was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer analysis (VSM), and X-ray photoelectron spectroscopy (XPS), and was used as a cleanup adsorbent in magnetic solid-phase extraction (MSPE) for determination of 15 trace-level environmental phenols in seafood coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS). The obtained results showed that the GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. The cleanup mechanisms were investigated and referred to π-π stacking interaction and hydrogen bond between GOE-CS-MM and impurities in the extracts. Moreover, the extraction and cleanup conditions of GOE-CS-MM toward phenols were optimized in detail. Under the optimized conditions, the limits of detection (LODs) were found to be 0.003-0.06 µg kg(-1), and satisfactory recovery values of 84.8-103.1% were obtained for the tested seafood samples. It was confirmed that the developed method is simple, fast, sensitive, and accurate for the determination of 15 trace environmental phenols in seafood samples.
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Contaminantes Ambientales/análisis , Grafito/química , Imanes , Microesferas , Óxidos/química , Fenoles/análisis , Alimentos Marinos/análisis , Cromatografía Liquida , Espectrometría de Masas en TándemRESUMEN
A planar graphene oxide-based magnetic ionic liquid nanomaterial (PGO-MILN) was synthesized. The prepared PGO-MILN was characterized by transmission electronmicroscopy (TEM) and Fourier-transform infrared spectrometry (FTIR). The results of adsorption experiments showed that the PGO-MILN had great adsorption capacity for 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP). Based on the adsorption experimental data, a sensitive magnetic method for determination of the five CPs in environmental water samples was developed by an effective magnetic solid-phase extraction (MSPE) procedure coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The effects of main MSPE parameters including the solution pH, extraction time, desorption time, and volume of desorption solution on the extraction efficiencies had been investigated in detail. The recoveries ranged from 85.3 to 99.3% with correlation coefficients (r) higher than 0.9994 and the linear ranges were between 10 and 500ngL(-1). The limits of detection (LODs) and limits of quantification (LOQs) of the five CPs ranged from 0.2 to 2.6ngL(-1) and 0.6 to 8.7ngL(-1), respectively. The intra- and inter- day relative standard deviations (RSDs) were in the range from 0.6% to 7.4% and from 0.7% to 8.4%, respectively. It was confirmed that the PGO-MILN was a kind of highly effective MSPE materials used for enrichment of trace CPs in the environmental water.
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Clorofenoles/análisis , Cromatografía Líquida de Alta Presión , Grafito/química , Líquidos Iónicos/química , Nanoestructuras/química , Espectrometría de Masas en Tándem , Contaminantes Químicos del Agua/análisis , Adsorción , Óxido Ferrosoférrico/química , Concentración de Iones de Hidrógeno , Límite de Detección , Magnetismo , Microscopía Electrónica de Transmisión , Óxidos/química , Dióxido de Silicio/química , Extracción en Fase Sólida , Espectroscopía Infrarroja por Transformada de Fourier , Contaminantes Químicos del Agua/aislamiento & purificaciónRESUMEN
Microcystins (MCs), a group of cyclic heptapeptide heaptoxins and tumor promoters, are generated by cyanobacteria occurring in surface waters, such as eutrophic lakes, rivers, and reservoirs. In this present study, a novel double-sided magnetic molecularly imprinted polymer modified graphene oxide (DS-MMIP@GO) based magnetic solid-phase extraction (MSPE) method was developed for fast, effective and selective enrichment, and recognition of trace MCs in environmental water samples combined with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The synthesized novel DS-MMIP@GO was used as the adsorbents in this work and was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and Raman spectra. The adsorption and desorption conditions of DS-MMIP@GO toward MCs were optimized in detail to obtain the highest binding capacity, selectivity, and release efficiency. Under the optimum conditions, the enrichment factors of the method for eight target MCs were found to be 2000. The limits of quantitation (LOQs) of the method for eight MCs were in range of 0.1-2.0ngL(-1). The double-sided MMIP modified structure provided DS-MMIP@GO with abundant adsorption sites and permitted it to exhibit excellent enrichment and selectivity toward trace-level MCs. The proposed method was successfully applied for the analysis of environmental water samples with recoveries ranging from 84.1 to 98.2%. Compared to conventional methods for MCs detection reported in literatures, the one developed in this work based on DS-MMIP@GO and LC-MS/MS showed much faster, more sensitive, and more convenient.
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Cromatografía Liquida , Monitoreo del Ambiente/métodos , Agua Dulce/química , Microcistinas/análisis , Microcistinas/aislamiento & purificación , Óxidos/química , Espectrometría de Masas en Tándem , Grafito/química , Magnetismo , Microscopía Electrónica de Transmisión , Polímeros/química , Extracción en Fase Sólida , Espectroscopía Infrarroja por Transformada de Fourier , Contaminantes Químicos del Agua/análisisRESUMEN
In this study, a rapid and accurate ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method combined with dispersive micro-solid-phase extraction (d-µ-SPE) using a core-shell nanoring amino-functionalized magnetic polymer (CS-NR-MP) was established and validated to determine trace dicyandiamide (DCD) in powdered milk. The developed d-µ-SPE cleanup procedure can dramatically reduce the matrix in samples, and lead to a significant reduction in absolute matrix effects. Chromatographic separation was performed on an Acquity UPLC BEH Amide column by using water-acetonitrile (9:91, v/v) as the mobile phase within 2 min. DCD was quantitatively analyzed by using DCD-(15)N2(13)C2 as an internal standard. The results showed that the recoveries were between 99.8 and 105.6% with RSDs in the range of 0.5-4.9%. The target compound had good linearity in the range of 0.1-20.0 µg L(-1) with a correlation coefficient (r) of 0.9996. The limit of quantification (LOQ) was 0.06 µg kg(-1). This method can be used for the rapid and sensitive determination of ultratrace DCD residue in powdered milk samples.
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Cromatografía Liquida/métodos , Guanidinas/análisis , Magnetismo , Leche/química , Microextracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Animales , Límite de Detección , Polímeros , Polvos , Reproducibilidad de los ResultadosRESUMEN
A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0µg/L in wines and soft drinks. The developed M-dSPE UFLC-MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95-42.6µg/L), and erythrosine in one out of fifteen dry red wine samples (3.22µg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses.
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Bebidas Gaseosas/análisis , Cromatografía Liquida , Colorantes/análisis , Tecnología de Alimentos/métodos , Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Vino/análisis , China , Fenómenos MagnéticosRESUMEN
A novel, simple and sensitive method was developed for the simultaneous determination of 22 sulfonamides (SAs) in chicken breast muscle by using the dispersive micro-solid-phase extraction (d-µ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS). The excellent core-shell nanoring amino-functionalized superparamagnetic molecularly imprinted polymer (CS-NR-Mag-MIP) was used as sorbent, and the main factors affecting the extraction efficiency were investigated in detail. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9980. The mean recoveries were in the range of 85.0-112.2% at low, medium and high concentration levels (0.1, 1.0 and 5.0 ng/g). The intra-day and inter-day relative standard deviations (RSDs) were lower than 6.0% and 8.9%, respectively. The limits of quantification for the 22 SAs were between 0.013 and 0.099 ng/g. The developed d-µ-SPE-UFLC-MS/MS method had been successfully applied to the chicken breast muscle samples for food-safety risk monitoring in Zhejiang Province, China. The results showed sulfamethazine, sulfamethoxazole and sulfaquinoxaline in five out of three hundred collected samples were detected with concentrations of 0.418-2.28, 16.4 and 2.93 ng/g, respectively. It was confirmed that the CS-NR-Mag-MIP was a kind of highly effective d-µ-SPE materials used for the SAs analyses.
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Cromatografía Líquida de Alta Presión/métodos , Compuestos Férricos/química , Carne/análisis , Impresión Molecular/métodos , Músculo Esquelético/química , Sulfonamidas/análisis , Espectrometría de Masas en Tándem/métodos , Animales , Pollos , Microextracción en Fase Líquida/métodos , Nanopartículas de Magnetita/química , Nanopartículas de Magnetita/ultraestructura , Nanopartículas del Metal/química , Nanopartículas del Metal/ultraestructura , Polímeros/química , Factores de TiempoRESUMEN
A novel planar-structure amine-functional magnetic polymer modified graphene oxide nanocomposite (NH2-MP@GO) was synthesized. The properties were characterized by transmission electron microscopy (TEM) and Fourier-transform infrared spectrometry (FTIR). The obtained adsorption results showed that the NH2-MP@GO had great adsorptive ability toward five chlorophenols (CPs), including 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP). Based on these, an effective magnetic solid-phase extraction (MSPE) procedure coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the preconcentration and determination of the five CPs in environmental water samples was developed. Various experimental parameters that could affect the extraction efficiencies had been investigated in detail. Under the optimum conditions, the enrichment factors of the method for the target CPs were found to be 1000. The proposed method was successfully applied for the analysis of environmental water samples with recoveries ranging from 86.4 to 99.8% with correlation coefficients (R) higher than 0.9994. Good linearities were obtained ranging from 10 to 500ng/L for 2-CP, 5 to 500ng/L for 2,4-DCP, 2 to 500ng/L for 2,4,6-TeCP and 2,3,4,6-TeCP, and 1 to 500ng/L for PCP, respectively. The limits of quantitation for the five CPs were 0.6-9.2ng/L. It was confirmed that the planar-structure NH2-MP@GO was a kind of highly effective MSPE materials used for the trace CPs analyses.
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Aminas/química , Clorofenoles/análisis , Cromatografía Liquida/métodos , Óxidos/química , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Agua/química , Adsorción , Cromatografía Liquida/instrumentación , Grafito/química , Concentración de Iones de Hidrógeno , Límite de Detección , Fenómenos Magnéticos , Polímeros/química , Extracción en Fase Sólida/instrumentación , Espectrometría de Masas en Tándem/instrumentaciónRESUMEN
A novel, simple and sensitive method was developed for the simultaneous determination of eight phenolic environmental estrogens in blood by using the dispersive micro-solid-phase extraction (d-µ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS). The excellent nanomaterials tetraethylenepentamine-functionalized magnetic polymer was used as an adsorbent, and the main factors affecting the extraction efficiency were investigated in detail. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.999. The mean recoveries were in the range of 85.0-105.0%. The intra-day and inter-day relative standard deviations (RSDs) were lower than 4.9% and 5.2%, respectively. The limits of quantification for the eight phenolic environmental estrogens were between 0.075 and 0.42 µg L(-1). The developed method can be applied to the routine analyses for the determination of the eight phenolic environmental estrogens in blood samples.
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Disruptores Endocrinos/sangre , Contaminantes Ambientales/sangre , Estrógenos/sangre , Etilenodiaminas/química , Nanoestructuras/química , Fenoles/sangre , Adsorción , Animales , Cromatografía Liquida/métodos , Límite de Detección , Imanes , Polimerizacion , Rana catesbeiana , Reproducibilidad de los Resultados , Extracción en Fase Sólida/métodos , Espectrometría de Masas en TándemRESUMEN
A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in red wine. The effects of ion-suppressors, i.e., trifluoroacetic acid (TFA) and ammonium acetate (AmAc) on retention behavior of nine food additives in RP-HPLC separation were discussed in detail. The relationships between retention factors of solutes and volume percent of ion-suppressors in the mobile-phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, respectively. The results showed that the ion suppressors had not only an ion suppression effect, but also an organic modification effect on the acidic analytes. The baseline separation of nine food additives was completed by a gradient elution with acetonitrile-TFA(0.01%, v/v)-AmAc(2.5 mmol L(-1)) aqueous solution as the mobile phase. The recoveries were between 80.2 - 99.5% for all analytes with RSDs in the range of 1.5 - 8.9%. The linearities were in the range of 0.2 - 100.0 mg L(-1) with determination coefficients (r(2)) higher than 0.9991 for all analytes. The limits of quantification (LOQs) were between 0.53 - 0.99 mg L(-1). The applicability of the proposed method to detect and quantify food additives has been demonstrated in the analysis of 30 real samples.
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Acetatos/química , Cromatografía Líquida de Alta Presión/métodos , Cromatografía de Fase Inversa/métodos , Aditivos Alimentarios/análisis , Análisis de los Alimentos/métodos , Ácido Trifluoroacético/química , Vino/análisis , Aditivos Alimentarios/química , Aditivos Alimentarios/aislamiento & purificación , Límite de Detección , Modelos Lineales , Espectrofotometría Ultravioleta , Factores de TiempoRESUMEN
A series of ethylenediamine (EDA)-functionalized magnetic polymers (EDA-MPs) have been prepared via suspension polymerization with the usage amount of the functional monomer glycidylmethacrylate (GMA) varied during the suspension polymerization procedure. The EDA-MPs were characterized by transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), X-ray diffractometer (XRD), thermogravimetry and differential thermogravimetry analysis (TG-DTA), Fourier-transformed infrared spectroscopy (FTIR) and elementary analyzer (EA). The adsorption properties of the EDA-MPs for the removal of Cr(VI) in wastewater were deeply studied. The results showed the adsorption efficiency was highly pH dependent and decreased with the increasing of initial concentration of Cr(VI). The adsorption data taken at the optimized condition, i.e., 35 degrees C and pH of 2.5 were well fitted with the Langmuir isotherm. The maximum adsorption capacities (q(m)) of EDA-MPs to Cr(VI) were highly related to the contents of EDA-MPs, i.e., the q(m) of EDA-MPs to Cr(VI) calculated from the Langmuir isotherm increased from 32.15 to 61.35 mg g(-1) with the increasing of the usage amount of GMA. The adsorption kinetic data were modeled by the pseudo-second-order rate equation, and the adsorption of Cr(VI) by all the present EDA-MPs reached equilibrium in 60 min.