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1.
J Hazard Mater ; 465: 133468, 2024 Mar 05.
Article in English | MEDLINE | ID: mdl-38219584

ABSTRACT

Microporous organic networks (MONs) are highly porous materials that are particularly useful in analytical chemistry. However, the use of these materials is often limited by the functional groups available on their surface. Here, we described the polymerization of a sea urchin-like structure material at ambient temperature, that was functionalized with hydroxyl, carboxyl, and triazine groups and denoted as OH-COOH-MON-TEPT. A substantial proportion of OH-COOH-MON-TEPT was intricately decorated EDA-Fe3O4, creating a well-designed configuration (EDA-Fe3O4 @OH-COOH-MON-TEPT-EDC) for superior adsorption of the target analytes phenylurea herbicides (PUHs) via magnetic solid-phase extraction (MSPE). The proposed method showed remarkably low limits of detection ranging from 0.03 to 0.22 ng·L-1. Experimental investigations and theoretical analyses unveiled the adsorption mode between EDA-Fe3O4 @OH-COOH-MON-TEPT-EDC and PUHs. These findings establish a robust foundation for potential applications of EDA-Fe3O4 @OH-COOH-MON-TEPT-EDC in the analysis of various polar contaminants.

2.
Sep Purif Technol ; 305: 122517, 2023 Jan 15.
Article in English | MEDLINE | ID: mdl-36340050

ABSTRACT

Chloroquine phosphate (CQP) has been suggested as an important and effective clinical reliever medication for the 2019 coronavirus (COVID-19). Nevertheless, its excessive use will inevitably cause irreparable damage to the entire ecosystem, thereby posing a considerable environmental safety concern. Hence, the development of highly-efficient methods of removing CQP from water pollution sources, e.g., effluents from hospitals and pharmaceutical factories is significant. This study reported the fabrication of novel C-N bond linked conjugated microporous polymers (CMPs) (BPT-DMB-CMP) with multiple nitrogen-rich anchoring sites for the quick and efficient removal of CQP from aqueous solutions. The irreversible covalent C-N bond linked in the internal framework of BPT-DMB-CMP endowed it with good chemical stability and excellent adsorbent regeneration. With its predesigned functional groups (i.e., rich N-H bonds, triazine rings, and benzene rings) and large area surface (1,019.89 m2·g-1), BPT-DMB-CMP demonstrated rapid adsorption kinetics (25 min) and an extraordinary adsorption capacity (334.70 mg·g-1) for CQP, which is relatively higher than that of other adsorbents. The adsorption behavior of CQP on BPT-DMB-CMP corresponded with Liu model and mixed-order model. Based on the density functional theory (DFT) calculations, X-ray photoelectron spectroscopy (XPS), and adsorption comparisons test, the halogen bonding, and hydrogen bonding cooperates with π - π, C - H···π interactions and size-matching effect in the CQP adsorption system on BPT-DMB-CMP. The excellent practicability for the removal of CQP from real wastewater samples verified the prospect of practical application of BPT-DMB-CMP. BPT-DMB-CMP exhibited the application potentials for the adsorption of other antiviral drugs. This work opens up an efficient, simple, and high adsorption capacity way for removal CQP.

3.
Food Chem ; 383: 132396, 2022 Jul 30.
Article in English | MEDLINE | ID: mdl-35158132

ABSTRACT

Development of efficient and sensitive adsorbent for capturing phenoxy carboxylic acids (PCAs) from environmental and food samples is necessary because PCAs could threaten human health. Designing nanoparticle with multiple functional groups is beneficial to achieve the strong adsorption interaction and the specific recognition for target compound. In this paper, TpTGCl as an ionic covalent organic framework (ICOF), that could offer plenty of positive charges and hydrogen-bonding sites, was fabricated. TpTGCl achieved quicker, more sensitive enrichment for anionic PCAs. The analysis of binding affinity by density functional theory (DFT) demonstrated that PCAs bonded to TpTGCl primarily via electrostatic attraction, N  H···O and O  H···O, and C  H···π interaction. The quantitative approach indicated low limits of detection (0.016-0.036 ng·g-1 for rice and 0.43-0.78 ng·L-1 for water). Furthermore, successfully determining PCAs emitted from real samples indicated the applicability of TpTGCl.


Subject(s)
Herbicides , Oryza , Adsorption , Carboxylic Acids/analysis , Chromatography, High Pressure Liquid , Herbicides/analysis , Humans , Oryza/chemistry , Solid Phase Extraction , Water/chemistry
4.
Food Chem ; 361: 130018, 2021 Nov 01.
Article in English | MEDLINE | ID: mdl-34023690

ABSTRACT

Developing and establishing an efficient pre-treatment approach for the precise extraction of nitrated-polycyclic aromatic hydrocarbons (N-PAHs) from real-life samples is critical for ensuring their safety. In this study, a novel crystalline magnetic covalent organic framework with a grapevine structure not a single core-shell, Fe3O4@TAPT-DMTA-COF, was fabricated via chemical bonding. Unchanging the reticulated structure and high crystallinity of TAPT-DMTA-COF, the combination made this material possess not only simple operation via magnetic decantation but also remarkable chemical stability. Fe3O4@TAPT-DMTA-COF had a large surface area (1578.45 m2/g), and rich electronegative triazine-groups, which makes it become a superior magnetic enrichment material for trace N-PAHs. For N-PAHs analysis, low limits of detection (LODs) (1.43-17.24 ng/L), excellent relative standard deviations (RSDs ≤ 11.52%), and wide linearity (10-5000 ng/L) were obtained. Real-life applications based on this composite have been successfully explored by capturing the N-PAHs emitted from food and environmental samples.


Subject(s)
Food Analysis/methods , Metal-Organic Frameworks/chemistry , Polycyclic Aromatic Hydrocarbons/analysis , Solid Phase Extraction/methods , Coffee/chemistry , Density Functional Theory , Food Analysis/instrumentation , Gas Chromatography-Mass Spectrometry , Limit of Detection , Magnetite Nanoparticles/chemistry , Meat Products/analysis , Polycyclic Aromatic Hydrocarbons/chemistry , Polycyclic Aromatic Hydrocarbons/isolation & purification , Sensitivity and Specificity , Solid Phase Extraction/instrumentation , Triazines/chemistry , Water Pollutants, Chemical/analysis
5.
J Hazard Mater ; 403: 123917, 2021 02 05.
Article in English | MEDLINE | ID: mdl-33264969

ABSTRACT

Food and environmental safety issues attributable to the polybrominated diphenyl ethers (PBDEs) are gaining increasing attention, and these urge us to establish a high-performance sample-handling technique. In this study, an outstanding adsorption performance with short adsorption time (10 min) was achieved for PBDEs using a novel synthesized dispersive solid-phase extraction adsorbent, a reticulated covalent organic framework with N/O functional groups (i.e., imine linkage, triazine, and methoxy) (TAPT-DMTA-COF). By conducting sufficient experimentation and theoretical simulation on adsorption mechanism, the halogen bond between electronegative N/O atoms of TAPT-DMTA-COF and the electropositive Br atoms of PBDEs were observed to play a more pivotal role than π-π, C-H…π interactions, and hydrophobic effects. Furthermore, the positive linear relation between calculated adsorption energy and Br content directly clarified that enrichment behavior of PBDEs can be attributed to halogen bonding. These data implied that integrated nanostructure (i.e., N/O functional groups and reticulated architecture) effectively enhanced adsorption capacity. In case of PBDE analysis, this approach achieved excellent results with low limits of detection (0.03-0.13 ng L-1). Finally, the promising potential applications of aforementioned method were verified by spiking water, fish, and milk samples with PBDEs; good PBDEs recoveries were obtained.


Subject(s)
Halogenated Diphenyl Ethers , Metal-Organic Frameworks , Adsorption , Animals , Solid Phase Extraction , Triazines
6.
Food Chem ; 345: 128841, 2021 May 30.
Article in English | MEDLINE | ID: mdl-33360062

ABSTRACT

In this study, a novel porous composite (Fe3O4@TAPB-COF@ZIF-8) consisting of metal-organic and covalent organic frameworks was developed and applied to the magnetic solid-phase extraction (MSPE) of bisphenols. The extraction parameters such as the extraction time, solution pH, amounts of adsorbent, and ionic strength were investigated to obtain the best extraction conditions. By optimizing the MSPE, a convenient and sensitive analytical method was established in combination with high-performance liquid chromatography. The method achieved low detection limits (0.04-0.05 ng mL-1), wide linear range (0.25-1000 ng mL-1), good repeatability (1.20-4.30%), good reproducibility (1.34-4.03%), and satisfactory recoveries of four functional beverages (66.2-116.6%).


Subject(s)
Benzhydryl Compounds/analysis , Benzhydryl Compounds/isolation & purification , Beverages/analysis , Limit of Detection , Magnetic Phenomena , Metal-Organic Frameworks/chemistry , Phenols/analysis , Phenols/isolation & purification , Solid Phase Extraction/methods , Adsorption , Benzhydryl Compounds/chemistry , Chromatography, High Pressure Liquid , Ferrosoferric Oxide/chemistry , Osmolar Concentration , Phenols/chemistry , Porosity , Reproducibility of Results
7.
Food Chem ; 345: 128749, 2021 May 30.
Article in English | MEDLINE | ID: mdl-33302110

ABSTRACT

The development of sensitive method for analysis ofpesticide residue is of great significance to ensure food safety and promote globalization of food trade. An original method was proposed for analysis of phenoxy carboxylic acids (PCAs) pesticide in plant-derived food. To concentrate trace PCAs, the TAPT-DHTA-COF was fabricated by a facile room-temperature method and utilized as the solid phase extraction cartridge packing. The TAPT-DHTA-COF exhibited excellent adsorption capacity and recyclability towards PCAs. Theoretical simulation indicated that the adsorption of PCAs onto the TAPT-DHTA-COF was driven by hydrogen bond, halogen bond and π-π interaction. Using liquid chromatography tandem mass spectrometry for detection, good linearity ranged from 0.10 to 40 ng·g-1 and low limits of detection varied from 0.007 to 0.030 ng·g-1 were achieved for PCAs in rice, apple and greengrocery. The recoveries of PCAs from the spiked samples ranged from 81.2% to 107%. The reliability was verified by the accurate determination of certified reference materials.


Subject(s)
Carboxylic Acids/analysis , Food Analysis/methods , Food Contamination/analysis , Hydroxyl Radical/chemistry , Metal-Organic Frameworks/chemistry , Pesticide Residues/analysis , Plants, Edible/chemistry , Adsorption , Carboxylic Acids/chemistry , Carboxylic Acids/isolation & purification , Chromatography, Liquid , Limit of Detection , Pesticide Residues/chemistry , Pesticide Residues/isolation & purification , Reproducibility of Results , Solid Phase Extraction , Tandem Mass Spectrometry
8.
J Chromatogr A ; 1630: 461534, 2020 Sep 12.
Article in English | MEDLINE | ID: mdl-32950812

ABSTRACT

Novel core shell structured magnetic covalent organic frameworks were synthesized at room temperature and first applied in water samples for the enrichment of trace polybrominated diphenyl ethers (PBDEs) through magnetic solid-phase extraction. The prepared materials were characterized through transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, vibrating sample magnetometer and X-ray photoelectron spectroscopy. During adsorption, the parameters affecting extraction and desorption efficiency were further optimized. Combined gas chromatography and mass spectrometry (GC/MS) revealed that high enrichment factors (275-292), low limits of detection (0.12-0.38 ng·L-1), wide linear ranges (0.5-1000 ng·L-1), and good reproducibility (intra-day 1.40%-4.31% and inter-day 5.14%-9.12%) were obtained under optimal conditions. The method successfully detected PBDEs in different water samples.

9.
Anal Methods ; 12(19): 2434-2442, 2020 05 21.
Article in English | MEDLINE | ID: mdl-32930232

ABSTRACT

Covalent organic frameworks with tunable porous crystallinity and outstanding stability have recently exhibited fascinating pretreatment performance as solid-phase microextraction coatings. In this report, a ß-ketoenamine-linked covalent organic framework (TpPa-1) was successfully constructed through a Schiff-base-type reaction between 1,3,5-triformylphloroglucinol (Tp) and para-phenylenediamine (Pa-1). A TpPa-1 coating was then fabricated on a stainless-steel fiber for capturing trace synthetic musks. This TpPa-1 coating exhibited strong interaction with synthetic musks because of its hydrophobicity and π-π affinity. This TpPa-1-based solid-phase microextraction methodology, coupled with gas chromatography-tandem mass spectrometry, provided high enrichment factors (1214-12 487), wide linearity (0.5-1000 ng L-1), low limits of detection (0.04-0.31 ng L-1), and acceptable reproducibility (relative standard deviation, <10%) for nine synthetic musks. Recoveries at three spiked levels in three types of water samples were between 76.2% and 118.7%. These results indicated the promising applicability of the TpPa-1 as a solid-phase microextraction fiber coating for reliably detecting trace concentrations of synthetic musks in the environment.

10.
J Chromatogr A ; 1625: 461275, 2020 Aug 16.
Article in English | MEDLINE | ID: mdl-32709327

ABSTRACT

Efficient extraction of polar sulfonamides antibiotics from aqueous samples and food is very challenging, because they are hydrophilic, their concentration is very low, and the matrix is complex. Covalent organic frameworks (COFs), a novel porous organic material, have attracted great attention. In this work, the spherical triphenylbenzene-dimethoxyterephthaldehyde-COFs (TPB-DMTP-COFs) were synthesized by a simple room temperature method, and due to their attractive properties, such as high outstanding acid-base stability, large specific surface area, low skeletal density, inherent porosity and high crystallinity, so TPB-DMTP-COFs as ideal solid phase extraction adsorbents showed excellent adsorption performance for trace polar sulfonamides in food and water. TPB-DMTP-COFs were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and so on. The important parameters were optimized to improve the extraction efficiency of TPB-DMTP-COFs toward sulfonamides. Analysis of sulfonamides was performed by liquid chromatography-tandem mass spectrometry. The developed method based on TPB-DMTP-COFs material achieved low limits of detection (0.5-1.0 ng L-1), wide linearity (5-1000 ng L-1), and good repeatability (2.5%-8.7%). The possible extraction mechanism was also discussed. Finally, the method was successfully applied to the enrichment and detection of sulfonamides in environmental water samples and food samples. The present study indicated that TPB-DMTP-COFs had splendid prospects in highly sensitive analysis of other pollutants in complex matrix.


Subject(s)
Food Analysis , Metal-Organic Frameworks/chemistry , Solid Phase Extraction/methods , Sulfonamides/analysis , Tandem Mass Spectrometry/methods , Water Pollutants, Chemical/analysis , Adsorption , Animals , Chromatography, Liquid , Food Contamination/analysis , Milk/chemistry , Pork Meat/analysis , Porosity , Sulfonamides/chemistry , Water/chemistry
11.
Molecules ; 24(16)2019 Aug 12.
Article in English | MEDLINE | ID: mdl-31408943

ABSTRACT

A multi-residue method for the determination of 107 pesticide residues in wolfberry has been developed and validated. Similar pretreatment approaches were compared, and the linearity, matrix effect, analysis limits, precision, stability and accuracy were validated, which verifies the satisfactory performance of this new method. The LODs and LOQs were in the range of 0.14-1.91 µg/kg and 0.46-6.37 µg/kg, respectively. The recovery of analytes at three fortification levels (10 µg/kg, 50 µg/kg, 100 µg/kg) ranged from 63.3-123.0%, 72.0-118.6% and 67.0-118.3%, respectively, with relative standard deviations (RSDs) below 15.0%. The proposed method was applied to the analysis of fifty wolfberry samples collected from supermarkets, pharmacies and farmers' markets in different cities of Shandong Province. One hundred percent of the samples analyzed included at least one pesticide, and a total of 26 pesticide residues was detected in fifty samples, which mainly were insecticides and bactericide. Several pesticides with higher detection rates were 96% for acetamiprid, 82% for imidacloprid, 54% for thiophanate-methyl, 50% for blasticidin-S, 42% for carbendazim, 42% for tebuconazole and 36% for difenoconazole in wolfberry samples. This study proved the adaptability of the developed method to the detection of multiple pesticide residues in wolfberry and provided basis for the research on the risks to wolfberry health.


Subject(s)
Liquid-Liquid Extraction/methods , Lycium/chemistry , Pesticide Residues/isolation & purification , Benzimidazoles/isolation & purification , Carbamates/isolation & purification , Chromatography, High Pressure Liquid/methods , Humans , Neonicotinoids/isolation & purification , Nitro Compounds/isolation & purification , Nucleosides/isolation & purification , Pesticide Residues/classification , Tandem Mass Spectrometry/methods , Thiophanate/isolation & purification , Triazoles/isolation & purification
12.
Mikrochim Acta ; 186(2): 108, 2019 01 14.
Article in English | MEDLINE | ID: mdl-30637544

ABSTRACT

A magnetic covalent organic framework (Fe3O4@COF) with core-shell structure was fabricated at room temperature and used as an adsorbent for magnetic solid-phase extraction of polar endocrine-disrupting phenols (4-n-nonylphenol, 4-n-octylphenol, bisphenol A and bisphenol AF). The sorbent was characterized by transmission electron microscopy, FTIR, powder X-ray diffraction and other techniques. The main parameters governing the extraction efficiency were optimized. The phenols were quantified by HPLC with fluorometric detection. The method has attractive features such as low limits of detection (0.08-0.21 ng.mL-1), wide linear ranges (0.5-1000 ng.mL-1), and good repeatability (intra-day: 0.39%-4.99%; inter-day: 1.57%-5.21%). Satisfactory results were obtained when the developed method was applied to determine the four target pollutants in real world drink samples with spiked recoveries over the range of 81.3~118.0%. This indicates that the method is a powerful tool for the enrichment and determination of endocrine-disrupting phenols in drink samples. Graphical abstract A magnetite based covalent organic framework (Fe3O4@COFs) was synthesized with TPAB, TPA and Fe3O4. It was used for magnetic solid-phase extraction of endocrine-disrupting phenols from plastic-packaged tea drink samples coupled with liquid chromatography (LC) for determination.

13.
Mikrochim Acta ; 185(10): 450, 2018 09 12.
Article in English | MEDLINE | ID: mdl-30209670

ABSTRACT

A porphyrinic metal-organic framework (PCN-224) was fabricated and used as an adsorbent for solid-phase extraction of ultratrace levels of polar sulfonamide antibiotics from food and drinking waters. The PCN-224 was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and powder X-ray diffraction analyses. Parameters affecting the extraction efficiency were optimized. The sulfonamides were quantified by liquid chromatography-tandem mass spectrometry. Figures of merit include (a) low limits of detection (0.07-0.47 ng·L-1), (b) wide linear ranges (0.5-2000 ng·L-1), and (c) good repeatabilities (2.8%-6.7%) and reproducibilities (1.7%-5.1%). The method was successfully applied to the determination of sulfonamides in food and drinking water samples. Graphical abstract A Zr(IV)-based porphyrinic metal-organic framework (PCN-224) was synthesized from a Zr6 cluster and the H2TCPP ligand. It was used for solid-phase extraction of sulfonamides from food and drinking water samples coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination.

14.
Talanta ; 186: 561-567, 2018 Aug 15.
Article in English | MEDLINE | ID: mdl-29784402

ABSTRACT

Metal-organic nanotubes (MONTs) have great potential for solid phase microextraction (SPME) on account of high specific surface area, tunable pore sizes, and exceptional thermal and chemical stability. In this work, zinc (II)-based metal-organic nanotubes (Zn-MONTs) were used as an adsorbent for the SPME of nitro-polycyclic aromatic hydrocarbons (NPAHs) at trace levels from environmental water samples. Gas chromatography-mass spectrometry was used for sample analysis and key factors were investigated and optimized. Under optimal parameters, the developed method achieved low limits of detection (1.4-7.3 ng L-1), wide linear range (10-5000 ng L-1), and high enrichment factors (1510-17,684). In comparison to the PDMS and DVB/CAR/PDMS fiber for potential commercial use, the Zn-MONTs fiber obtained MS responses 2-9 times as high as those achieved by the commercial 100 µm PDMS and 0.2-2.3 times higher than 50/30 µm DVB/CAR/PDMS fiber did. The proposed method was successfully used in the analysis of NPAHs at trace levels in environmental samples.

15.
Molecules ; 23(4)2018 Apr 14.
Article in English | MEDLINE | ID: mdl-29661989

ABSTRACT

In this work, bamboo charcoal was used as solid-phase extraction adsorbent for the enrichment of six perfluoroalkyl acids (PFAAs) in environmental water samples before liquid chromatography-tandem mass spectrometry analysis. The specific porous structure, high specific surface area, high porosity, and stability of bamboo charcoal were characterized. Several experimental parameters which considerably affect extraction efficiency were investigated and optimized in detail. The experimental data exhibited low limits of detection (LODs) (0.01-1.15 ng/L), wide linear range (2-3 orders of magnitude and R ≥ 0.993) within the concentration range of 0.1-1000 ng/L, and good repeatability (2.7-5.0%, n = 5 intraday and 4.8-8.3%, n = 5 interday) and reproducibility (5.3-8.0%, n = 3). Bamboo charcoal was successfully used for the enrichment and determination of PFAAs in real environmental water samples. The bamboo charcoal-based solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry analysis possessed great potential in the determination of trace PFAA levels in environmental water samples.


Subject(s)
Charcoal/chemistry , Chromatography, Liquid/methods , Fluorocarbons/analysis , Poaceae/chemistry , Solid Phase Extraction/methods , Tandem Mass Spectrometry/methods , Water Pollutants, Chemical/analysis , Spectroscopy, Fourier Transform Infrared
16.
Anal Chim Acta ; 1015: 27-34, 2018 Jul 26.
Article in English | MEDLINE | ID: mdl-29530249

ABSTRACT

The high performance separation and pre-concentration of polar phenols from aqueous matrices is difficult because of the strong interactions between phenols and water molecules. Conjugated microporous polymers (CMPs) are a kind of novel porous organic materials. Polyphenylene core-conjugated microporous polymers (PPc-CMPs) were used as a novel coating material in the solid-phase microextraction of polar phenols in water samples for the first time. The novel PPc-CMPs fibers exhibited good thermal stability (>450 °C), high enrichment factors (519-2372), low limits of detection (0.02-0.05 ng L-1), wide linearity (0.1-1000 ng L-1), and good repeatability (2.5%-8.1%) for polar phenols. The new coating was successfully used in the analysis of phenols in real environmental water samples. PPc-CMPs as a polar solid-phase microextraction coating material was excellent for the rapid and sensitive analysis of phenols at trace levels in the environment.

17.
Anal Bioanal Chem ; 410(6): 1657-1665, 2018 Feb.
Article in English | MEDLINE | ID: mdl-29330603

ABSTRACT

Covalent organic frameworks (COFs), which are a new type of carbonaceous polymeric material, have attracted great interest because of their large surface area and high chemical and thermal stability. However, to the best of our knowledge, no work has reported the use of magnetic COFs as adsorbents for magnetic solid-phase extraction (MSPE) to enrich and determine environmental pollutants. This work aims to investigate the feasibility of using covalent triazine-based framework (CTF)/Fe2O3 composites as MSPE adsorbents to enrich and analyze perfluorinated compounds (PFCs) at trace levels in water samples. Under the optimal conditions, the method developed exhibited low limits of detection (0.62-1.39 ng·L-1), a wide linear range (5-4000 ng L-1), good repeatability (1.12-9.71%), and good reproducibility (2.45-7.74%). The new method was successfully used to determine PFCs in actual environmental water samples. MSPE based on CTF/Fe2O3 composites exhibits potential for analysis of PFCs at trace levels in environmental water samples. Graphical abstract Magnetic covalent triazine-based frameworks (CTFs) were used as magnetic solid-phase extraction adsorbents for the sensitive determination of perfluorinated compounds in environmental water samples. PFBA perfluorobutyric acid, PFBS perfluorobutane sulfonate, PFDA perfluorodecanoic acid, PFDoA perfluorododecanoic acid, PFHpA perfluoroheptanoic acid, PFHxA perfluorohexanoic acid, PFHxS perfluorohexane sulfonate, PFNA perfluorononanoic acid, PFOA perfluorooctanoic acid, PFPeA perfluoropentanoic acid, PFUdA Perfluoroundecanoic acid.

18.
J Sep Sci ; 40(8): 1755-1764, 2017 Apr.
Article in English | MEDLINE | ID: mdl-28217859

ABSTRACT

Aminosilanized magnetic carbon microspheres as a novel adsorbent were designed and fabricated. The adsorbent was used for the magnetic solid-phase extraction of bisphenols at trace levels from environmental water samples before liquid chromatography with tandem mass spectrometry analysis. The structure, surface, and magnetic behavior of the as-prepared aminosilanized magnetic carbon microspheres were characterized by elemental analysis, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, and vibrating sample magnetometry. The effects of the experimental parameters were investigated by the Plackett-Burman design, and then the parameters that were significant to the extraction efficiencies were optimized through a response surface methodology. The aminosilanized magnetic carbon microspheres exhibited high adsorption efficiency and selectivity for bisphenols. Under optimal conditions, low limits of detection (0.011-2.22 ng/L), and a wide linear range (2-3 orders of magnitude), good repeatability (4.7-7.8%, n = 5), and reproducibility (6.0-8.3%, n = 3) were achieved. The results demonstrate that the novel adsorbent possesses great potentials in the determination of trace levels of bisphenols in environmental water samples.

19.
Anal Bioanal Chem ; 408(29): 8289-8297, 2016 Nov.
Article in English | MEDLINE | ID: mdl-27704175

ABSTRACT

In this study, stable cadmium(II)-based metal-organic nanotubes (Cd-MONTs) were prepared and used as a coating material for solid-phase microextraction (SPME) of polychlorinated biphenyls (PCBs) from environmental water samples. The as-prepared Cd-MONT SPME coating material was characterized by thermal gravimetric analysis, scanning electron microscopy, and X-ray diffraction. The synthesized Cd-MONTs exhibited high thermal stability (385 °C) and excellent extraction performance toward PCBs. The important conditions were optimized systematically by the response surface method. Under the optimal conditions, the new fiber achieved high enrichment factors (938-3417), low limits of detection (1.80-8.73 pg L-1), and wide linearity (10-5000 pg L-1). The method developed was used in ultratrace-level analysis of PCBs in seawater samples, with satisfactory results for each sample.

20.
J Chromatogr A ; 1449: 39-47, 2016 Jun 03.
Article in English | MEDLINE | ID: mdl-27156750

ABSTRACT

A new type of three-dimensional, echinus-like magnetic Fe3O4 @ cobalt(Ⅱ)-based metal-organic nanotube (Fe3O4 @ Co-MONT) yolk-shell microspheres, have been designed and synthesized for the first time. Fe3O4 @ Co-MONTs yolk-shell microspheres were characterized by scanning electron micrographs, transmission electron microscopy, Fourier transform infrared spectra, X-ray diffraction, and vibrating sample magnetometry. The feasibility of the new material for use as an absorbent was investigated for magnetic solid phase-extraction (MSPE) of polychlorinated biphenyls (PCBs) from environmental water samples and biological samples. The Plackett-Burman design and Box-Behnken design were used to determine and optimize the extraction parameters influencing the extraction efficiency through response surface methodology. Under the optimized conditions, the developed method showed good linearity within the range of 5-1000ngL(-1), low limits of detection (0.31-0.49ngL(-1)), and good reproducibility (RSD<10%). The proposed method was successfully applied for the analysis of PCBs in real environmental water samples. These results demonstrated that Fe3O4 @ Co-MONTs is a promising adsorbent material for the MSPE of PCBs at trace levels from environmental water samples and biological samples.


Subject(s)
Cobalt/chemistry , Environmental Pollutants/isolation & purification , Ferrosoferric Oxide/chemistry , Organometallic Compounds/chemistry , Polychlorinated Biphenyls/isolation & purification , Animals , Cattle , Environmental Pollutants/blood , Environmental Pollutants/urine , Fresh Water/chemistry , Gas Chromatography-Mass Spectrometry/methods , Microspheres , Nanotubes , Polychlorinated Biphenyls/blood , Polychlorinated Biphenyls/urine , Reproducibility of Results , Solid Phase Extraction/methods , Wastewater/chemistry
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