scholarly journals NH2-MIL-53(Al) Polymer Monolithic Column for In-Tube Solid-Phase Microextraction Combined with UHPLC-MS/MS for Detection of Trace Sulfonamides in Food Samples

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 897 ◽  
Author(s):  
Qian-Chun Zhang ◽  
Guang-Ping Xia ◽  
Jun-Yi Liang ◽  
Xiao-Lan Zhang ◽  
Li Jiang ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Solid Phase Microextraction ◽  
In Situ Polymerization ◽  
Solid Phase ◽  
Monolithic Column ◽  
Metal Organic Framework ◽  
Food Samples ◽  
X Ray ◽  
Polymer Monolithic Column ◽  
Relative Standard

In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.

Pillarene functionalized polymer monolithic column for the solid-phase microextraction preconcentration of parabens

RSC Advances ◽  
2014 ◽  
Vol 4 (90) ◽  
pp. 49153-49160 ◽  
Author(s):  
Dan Liu ◽  
Nan Song ◽  
Ye-Chun Cheng ◽  
Dai-Xiong Chen ◽  
Qiong Jia ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Monolithic Column ◽  
Polymer Monolithic Column

Fluorescence Enhancement Method for Enrofloxacin Extraction by Core–Shell Magnetic Microspheres

2020 ◽  
Vol 73 (11) ◽  
pp. 1105
Author(s):  
Linyan Yang ◽  
Leiming Fu ◽  
Boxin Li ◽  
Jifei Ma ◽  
Cun Li ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Metal Organic Framework ◽  
Sodium Dodecyl ◽  
Covalent Modification ◽  
Magnetic Microspheres ◽  
Magnetic Characteristics ◽  
Fluorescent Properties ◽  
Xps Spectra ◽  
X Ray

In this work, we present novel kinds of γ-Fe2O3@SiO2-NH2-CMC/MOF5 and γ-Fe2O3@SiO2-NH2-CMC/IRMOF3 magnetic metal–organic framework (MOF) nanoparticles which possess both magnetic characteristics and fluorescent properties. Here, [Zn4O(bdc)3] (MOF-5, bdc=1,4-benzenedicarboxylate) is a kind of shell. IRMOF3, a known MOF with a cubic topology prepared from Zn(NO3)2⋅4H2O and 2-amino-1,4-benzene dicarboxylic acid, is another kind of shell which is attractive due to its highly porous, crystalline structure and the presence of non-coordinating amino groups on the benzenedicarboxylate (bdc) linker, which are amenable to post-synthetic modification. γ-Fe2O3@SiO2-NH2-CMC magnetic nanoparticles (MNPs) could be prepared by covalent modification of sodium carboxymethyl cellulose (CMC). The structure of γ-Fe2O3 nanoparticles could be determined by X-ray powder diffraction (XRD). X-ray photoelectron spectroscopy (XPS) spectra could be used for the characterisation of γ-Fe2O3@SiO2-NH2, γ-Fe2O3@SiO2-NH2-CMC, γ-Fe2O3@SiO2-NH2-CMC/MOF5, and γ-Fe2O3@SiO2-NH2-CMC/IRMOF3 nanoparticles. Magnetic solid-phase extraction (MSPE) of enrofloxacin (Enr) experiments exhibited that, for γ-Fe2O3@SiO2-NH2-CMC/IRMOF3, the best effects of adsorption could be obtained at pH 4 and 6, while elution conditions of 0.1mol L−1 NaOH and 1% sodium dodecyl sulfate could achieve the best elution effect. The addition of Tb3+ ions could sensitise the fluorescence of Enr. At the same time, via the addition of Tb3+ ions, coordination could occur between nanoparticles and Tb3+ ions, which could be verified by XPS.

scholarly journals Poly (Octadecyl Methacrylate-Co-Trimethylolpropane Trimethacrylate) Monolithic Column for Hydrophobic in-Tube Solid-Phase Microextraction of Chlorophenoxy Acid Herbicides

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1678 ◽  
Author(s):  
Wenbang Li ◽  
Fangling Wu ◽  
Yongwei Dai ◽  
Jing Zhang ◽  
Bichen Ni ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Monolithic Column ◽  
Pollution Source ◽  
Hplc Method ◽  
Rice Grains ◽  
Relative Standard ◽  
Chlorophenoxy Acid Herbicides ◽  
Highly Hydrophobic ◽  
Acid Herbicides

Chlorophenoxy acid herbicides (CAHs), which are widely used on cereal crops, have become an important pollution source in grains. In this work, a highly hydrophobic poly (octadecyl methacrylate-co-trimethylolpropane trimethacrylate) [poly (OMA-co-TRIM)] monolithic column has been specially prepared for hydrophobic in-tube solid-phase microextraction (SPME) of CAHs in rice grains. Due to the hydrophobicity of CAHs in acid conditions, trace CAHs could be efficiently extracted by the prepared monolith with strong hydrophobic interaction. Several factors for online hydrophobic in-tube SPME, including the length of the monolithic column, ACN and trifluoroacetic acid percentage in the sampling solution, elution volume, and elution flow rate, were investigated with respect to the extraction efficiencies of CAHs. Under the optimized conditions, the limits of detection of the four CAHs fell in the range of 0.9–2.1 μg/kg. The calibration curves provided a wide linear range of 5–600 μg/kg and showed good linearity. The recoveries of this method ranged from 87.3% to 111.6%, with relative standard deviations less than 7.3%. Using this novel, highly hydrophobic poly (OMA-co-TRIM) monolith as sorbent, a simple and sensitive online in-tube SPME-HPLC method was proposed for analysis of CAHs residue in practical samples of rice grains.

scholarly journals Development of ultrasound-assisted dispersive solid-phase microextraction based on mesoporous carbon coated with silica@iron oxide nanocomposite for preconcentration of Te and Tl in natural water systems

2020 ◽  
Vol 18 (1) ◽  
pp. 412-425
Author(s):  
Luthando Nyaba ◽  
Buyile Dubazana ◽  
Anele Mpupa ◽  
Philiswa N. Nomngongo
Keyword(s):  
Electron Microscopy ◽  
Inductively Coupled Plasma ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Sol Gel ◽  
Emission Spectrometry ◽  
X Ray ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Ultrasound Assisted

AbstractThe main objective of this study was to develop an ultrasound-assisted dispersive solid-phase microextraction (UADSPME) method for separation and preconcentration of tellurium (Te) and thallium (Tl) in environmental samples prior to inductively coupled plasma-optical emission spectrometry determination. The MPC@SiO2@Fe3O4 nanocomposite was used as a nanoadsorbent in the UADSPME method. The nanocomposite was prepared using a coprecipitation and sol–gel method, and it was characterized using scanning electron microscopy/energy-dispersive X-ray spectroscopy, transmission electron microscopy and X-ray powder diffraction techniques. The Box–Behnken design and response surface methodology were used for the optimization of experimental parameters (such as pH, extraction time and mass of adsorbent) affecting the preconcentration procedure. Under optimized conditions, the limits of detection were 0.05 and 0.02 µg L−1 and the limits of quantification were 0.17 and 0.07 µg L−1 for Te and Tl, respectively. The precision expressed as the relative standard deviation (%RSD) was 2.5% and 2.8% for Te and Tl, respectively. Finally, the developed method was applied for the analysis of Tl and Te in real samples.

scholarly journals Carbonized Aramid Fiber as the Adsorbent for In-Tube Solid-Phase Microextraction to Detect Estrogens in Water Samples

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Xiaoxiao Zhu ◽  
Yijun Zhang ◽  
Pengfei Liu ◽  
Xiuzhi Bai ◽  
Na Chen ◽  
...  
Keyword(s):  
Water Samples ◽  
Photoelectron Spectroscopy ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Sampling Rate ◽  
Steel Tube ◽  
Aramid Fiber ◽  
Stainless Steel Tube ◽  
Raman Spectrometry ◽  
Relative Standard

Carbonized aramid fiber was prepared as a new type of adsorbent for in-tube solid-phase microextraction. The surface structure, chemical composition, and graphitization degree of the resulted fiber was determined and characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, and Raman spectrometry. The prepared fiber was packed in a stainless-steel tube instead of the sample loop of a six-port and tested for the extraction of five environmental estrogen hormones coupled with high-performance liquid chromatography. Several parameters affecting the estrogens’ extraction including the sampling volume, sampling rate, NaCl content, and desorption time were investigated in detail. The extraction tube with carbonized aramid fiber exhibited remarkable extraction performance towards five estrogen targets. The analysis method was established, and it exhibited a wide linear range (0.5–10.0 μg/L) with good linearity (correlation coefficient ≥0.9906), low limits of detection (0.011–0.13 μg/L), and high enrichment factors (178–1335) for the five analytes. Relative standard deviations (n = 3) for intraday (≤4.8%) and interday (≤4.0%) tests indicated that the extraction material had satisfactory repeatability. Bisphenol A released from a polycarbonate (PC) bottle was quantitatively detected with a concentration of 8.3 μg/L. The relative recoveries spiked at 5 and 10 μg/L were investigated, and the results were in the range of 74.3–121% for real water samples.

scholarly journals Ultrasound-assisted dispersive micro-solid phase extraction using molybdenum disulfide supported on reduced graphene oxide for energy dispersive X-ray fluorescence spectrometric determination of chromium species in water

2020 ◽  
Vol 187 (9) ◽  
Author(s):  
Katarzyna Pytlakowska ◽  
Karina Kocot ◽  
Michał Pilch ◽  
Maciej Zubko
Keyword(s):  
Electron Microscopy ◽  
Graphene Oxide ◽  
Molybdenum Disulfide ◽  
Photoelectron Spectroscopy ◽  
Solid Phase ◽  
Sample Volume ◽  
Aqueous Sample ◽  
X Ray ◽  
Chromium Vi ◽  
Relative Standard

Abstract Molybdenum disulfide (MoS2) was supported on graphene oxide (GO) by hydrothermal method. The resulting nanocomposite (MoS2-rGO) was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The experiments show that at pH 2, MoS2-rGO has a great affinity for adsorption of hexavalent chromium ions while Cr(III) ions remain in aqueous sample. In the adsorption process, the dominant role plays chemisorption. The determined adsorption capacity is 583.5 mg g−1. Parameters affecting the extraction process, namely sample pH, sample volume, contact time, and matrix ions, were investigated by sequential batch tests. Under optimal conditions (pH 2, sample volume 50 mL, sonication time 10 min, adsorbent mass 1 mg), the calibration curve covers the 1–200 ng mL−1 range with a correlation coefficient (R2) of 0.998. The recovery of the method is 97 ± 3%. Other data of merit include a relative standard deviation of < 3.5%, enrichment factor of 3350, and detection limit of 0.050 ng mL−1. The accuracy of the method was confirmed by analysis of the reference materials QC1453 (chromium VI in drinking water) and QC3015 (chromium VI in seawater). The method was successfully applied to chromium speciation in water samples, including high salinity ones. The concentration of Cr(III) was calculated as the difference between the total concentration of chromium (after oxidation of Cr(III) to Cr(VI) with potassium permanganate) and the initial Cr(VI) content. Graphical abstract

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