ANALYTICAL LETTERS
·
2022
·
IF 2.267
Lanying Xu,Yingying Huang,Bingshan Zhao,Limin Ren,Tao Long
β-Cyclodextrin modified magnetic microspheres were synthesized and used as an effective adsorbent for the solid-phase extraction of three phenols from water samples. Scanning electron microscopy and Fourier transform infrared spectrometry were used to characterize the adsorbents. The major parameters affecting the extraction and desorption efficiencies, such as adsorbent dosage, extraction time, pH, ionic strength, and eluent type were systematically optimized. Under these conditions, three phenols in water samples were extracted and determined by high performance liquid chromatography (HPLC) with diode array detection (DAD). Limits of detection (LODs) of 0.04–0.34 ng mL−1 and limits of quantification (LOQs) from 0.13 to 1.14 ng mL−1 were achieved with good repeatability (relative standard deviation <7.5%). The developed method was applied for the determination of 2,4-dichlorophenol, 2,4-dinitrophenol and bisphenol A in spiked Yangtze River water, and the recoveries were from 81.0% to 94.9%. The results demonstrated that the combination of magnetic solid-phase extraction (MSPE) with HPLC-DAD is suitable for the determination of trace phenolics in environmental water.
研究领域:
环境科学
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分析化学
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水质分析
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Jia-Hui Zhu,Sheng-Nan Lyu,Mo-Lin Li,Yu-Shen Liu,Lu-Liang Wang
Avermectins (AVMs) are widely used as broad-spectrum and potent antiparasitic activities. The AVMs residual in animal-derived products and poses potential risks to human health through the food chain. Existing detection methods struggle with ultra-trace residues and matrix interferences in complex samples, necessitating efficient sample pretreatment techniques. This study introduces a novel one-pot in situ synthesis of magnetic covalent organic framework (COF) nanoflowers (Fe 3 O 4 @TFB-TAPA) at room temperature, leveraging a green strategy that eliminates toxic solvents and high-pressure conditions. The unique Fe 3 O 4 @TFB-TAPA nanoflower enhanced surface area and adsorption efficiency, and were comprehensively characterization using XRD, FT-IR, TEM, VSM and TGA. Critical parameters for magnetic solid-phase extraction (MSPE) were optimized. The MSPE protocol was coupled with HPLC-FLD for sensitive detection. The Fe 3 O 4 @TFB-TAPA exhibited exceptional performance: high adsorption capacity due to π-π stacking and hydrogen bonding, superparamagnetic behavior and thermal stability. The method achieved rapid extraction within 5 min and low solvent consumption. Method validation showed wide linear ranges (0.2–600 ng/mL), low detection limits (0.06 ng/mL), and high precision (RSD < 5 %). Reusability exceeded 7 cycles with 96.5 % recovery.
研究领域:
分析化学
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环境科学
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食品安全
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纳米材料
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分离科学
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DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2025
·Vol. 192
·期 11
·1-18
·
IF 5.3
Xie Kexin,Wang Chunfeng,Pang Ningjia,Cheng Yanan,Chen Mengyi,Mu Taotao,Xiao Deli,Di Bin
The design and synthesis of Fe 3 O 4 @PDA@poly(AA-co-EGDMA) nanoparticles (NPs) as a novel magnetic solid-phase extraction (MSPE) material for efficient enrichment and detection of synthetic cannabinoids (SCs) of various structures in large-volume wastewater is reported. The Fe 3 O 4 @PDA@poly(AA-co-EGDMA) NPs were synthesized via a two-step process involving dopamine polymerization and functionalization with poly(acrylic acid-co-ethylene glycol dimethacrylate) polymers, providing hydrophobic and acidic functional groups for enhanced analyte adsorption. An MSPE-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the detection of 24 SCs in wastewater. The method exhibited excellent analytical performance with good linearity ( R > 0.99), low limits of quantification (LOQ, 0.02–0.1 ng/L), and good precision with recoveries ranging from 50.20 to 92.72%. The method is capable of reliably analyzing trace SCs in large volume samples (300 mL and 1 L). This study introduces a simple, rapid, and cost-effective MSPE-UPLC-MS/MS approach for detecting SCs in complex environmental samples. The proposed method offers significant potential for wastewater-based epidemiology (WBE) applications, providing a valuable tool for monitoring drug use trends, public health surveillance, and regulatory enforcement. Graphical
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PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2020
·Vol. 34
·期 10
·e8742
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IF 2.2
Jichao Liu,Guoliang Li,Di Wu,Yanxin Yu,Jian Chen,Yongning Wu
Rationale Sedatives, which are prone to cause residues in animals, have been abused in modern animal husbandry. Long-term consumption of contaminated meat products would be unfavorable to the human nervous system. Taking into account public health and food safety, it was essential to develop an effective method for the enrichment and detection of sedatives in meat. Methods Fe 3 O 4 @TbBd@ZIF-8 composites were synthesized by using Fe 3 O 4 nanoparticles as a magnetic core and 1,3,5-triformylbenzene (Tb) and benzidine (Bd) as two building blocks to form Fe 3 O 4 @TbBd. Furthermore, the zeolitic imidazolate framework-8 (ZIF-8) was modified on the surface of the Fe 3 O 4 @TbBd. In addition, Fe 3 O 4 @TbBd@ZIF-8 was used as a magnetic solid-phase extraction (MSPE) adsorbent of typical animal sedatives in pork samples. Mass spectrometry analysis was conducted by electrospray ionization triple-quadrupole mass spectrometry in positive-ion multiple reaction monitoring mode. Results By combining the optimized MSPE approach with high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), an accurate and sensitive method for the determination of sedatives was developed. The method exhibited good linearity in the range of 0.03–70 μg/kg with the correlation coefficient (R 2 ) ranging from 0.9982 to 0.9999, high sensitivity with limits of detection (LODs) ranging from 0.04 to 0.2 μg/kg, and high precision with relative standard deviation (RSD) less than 5.5%. The adsorption behaviors of Fe 3 O 4 @TbBd@ZIF-8 towards sedatives were more suitably described by a pseudo-second-order kinetic and Freundlich isotherm model. Conclusions The proposed MSPE-HPLC/MS/MS method was successfully applied to the determination of sedatives in real samples and showed excellent applicability. Several sedatives were detected in the selected meat samples. The developed method was shown to be facile, sensitive and accurate for sedative detection and also showed great prospects for determination of sedatives from other complex samples.
研究领域:
分析化学
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食品安全
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材料科学
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DOI
PubMed
高影响因子
RSC Advances
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2022
·Vol. 12
·期 12
·7253-7261
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IF 4.036
Yuxin Liu,Wei Song,Dianbing Zhou,Fang Han,Xiaoming Gong,Pan Pan
In this study, a new core–shell magnetic mesoporous surface molecularly imprinted polymer (Fe3O4@SiO2@mSiO2-MIPs) which has specific adsorption and rapid adsorption rate for phthalate esters (PAEs) was prepared by a convenient method. Based on this composite as a magnetic solid phase extraction (MSPE) material, a rapid, efficient and sensitive matrix dispersion magnetic solid-phase extraction gas chromatography-mass spectrometry method (DMSPE-GC/MS) was developed for the determination of PAEs in multiple liquid samples. It is the first time that Fe3O4@SiO2@mSiO2-MIPs have been prepared by bonding amino groups on the surface of a double layer silicon substrate with diisononyl phthalate (DINP) as virtual template and 3-(2-aminoethyl)-aminopropyl trimethoxymethylsilane (TSD) as functional monomer. FT-IR, TEM, EDS, SEM, XRD, BET and VSM were used to characterize the composite. The adsorption isotherm and kinetics of Fe3O4@SiO2@mSiO2-MIPs showed that it possessed fast adsorption rates (approximately 5 min to reach equilibrium), high adsorption capacities (523.9 mg g−1) and good recognition of PAEs. The real samples were preconcentrated by Fe3O4@SiO2@mSiO2-MIPs, under the optimum DMSPE-GC/MS conditions. Validation experiments showed that the method presented good linearity (R2 > 0.9971), satisfactory precision (RSD < 5.7%) and high recovery (92.1–105.8%), and the limits of detection ranged from 1.17 ng L−1 to 3.03 ng L−1. The results indicated that the novel method had good sensitivity, high efficiency and wide sample application and was suitable for the determination of PAEs in liquid drink samples such as water, alcohol, beverages and so on.
研究领域:
分析化学
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环境科学
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DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2025
·
IF 6
Feng Zhang,Sen Zhang,Xing Liu,Wei Gao,Jun Luo,Yi-fan Pan,Wei-Juan Zheng,Xin Hu,Hong-zhen Lian
Background Glycoproteins are critical in various biological processes and attract lots of attention of researchers. It still remains a challenge to detect glycopeptides by mass spectrometry because of their low abundance with heterogeneity and lability, as well as signal suppression by non-glycopeptides. The boronate affinity-based enrichment is an effective solution for detecting cis -diols-containing compounds including glycopeptides in complex matrices. However, there has not been any report about absolute quantitation of boron in the absorbent materials for glycopeptides, which obstructed the tailored design of boronate affinity materials and deeper understanding of interaction mechanisms. Results This work presents the development of a boronic acid-functionalized magnetic zirconium metal-organic framework (mMOF–AAPBA) with actual boron content for specific capture of glycopeptides. The synthesized nanocomposite could enrich glycopeptides by magnetic solid-phase extraction (MSPE) via the synergistic effect of hydrophilic interaction and boronate affinity. After full characterization including quantitative analysis of boron by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), mMOF–AAPBA was applied as MSPE absorbent to capture glycopeptides. Under the optimized conditions, it could enrich 28 glycopeptides both from horseradish peroxidase and immunoglobulin digests, with a limit of detection of 1 fmol μL −1 coupled with matrix-assisted laser desorption/ionization time of flight mass spectrometry. The boronate affinity absorbent also possessed great ability of anti-interference and good reusability. Furthermore, it possessed high performance in enriching glycopeptides in real samples including human saliva and traditional Chinese medicine injections. Significance In the preparation of the boron-containing nanocomposites, there is a special interest that an accurate protocol was established to assay boron based on LA-ICP-MS assisted by home-made matrix reference substances for the first time. These findings highlight the quantitative boron-containing mMOF–AAPBA as a robust affinity material for glycopeptide enrichment in real biological samples, offering potential applications in glycoproteomics and other cis -diols compound related researches.
研究领域:
分析化学
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生物化学
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纳米技术
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质谱学
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糖蛋白质组学
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PubMed
高影响因子
MICROCHIMICA ACTA
·
2014
·Vol. 182
·期 3
·737-744
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IF 3.719
Yang Jing,Si Ling,Cui Shihai,Bi Wentao
We have developed a facile in-situ growth method for the deposition of magnetite (Fe 3 O 4 ) particles on the surface of a graphitic carbon nitride (g-C 3 N 4 ) nanosheet. The material was characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The high affinity of g-C 3 N 4 for phenolic acids in combination with the magnetism of Fe 3 O 4 provides an efficient means for magnetic solid phase extraction. The adsorption, desorption and recoveries were examined. Under optimized conditions, the method has limits of detection in the range from 17.5–42.6 ng mL −1 (at an S/N of 3), and precisions from 2.8–3.8 % (for n = 5). The method was successfully applied to the determination of protocatechuic, caffeic, and ferulic acids in Salicornia herbacea L . plant extracts. Recoveries ranged from 92.4–99.5 %.
The high affinity of g-C 3 N 4 toward the phenolic acids as well as the magnetic behavior of Fe 3 O 4 were combined in this nanocomposite material to provide an efficient and simple magnetic solid phase extraction (MSPE) approach.
研究领域:
材料科学
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分析化学
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环境科学
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DOI
高影响因子
TALANTA
·
2019
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IF 4.916
Yalin Wu,Qingxiang Zhou,Yongyong Yuan,Hongyuan Wang,Yayan Tong,Yali Zhan,Xueying Sheng,Yi Sun,Xianqi Zhou
Phthalate esters (PAEs) are an important kind of environmental endocrine disrupting chemicals , and have attracted great attention in environmental field. Present study described a new method for rapid and sensitive determination of PAEs including dibenzyl phthalate (DPhP), dibutyl phthalate (DnPP), and dicyclohexyl phthalate (DCHP) from aqueous matrices based on magnetic solid-phase extraction. Polyamidoamine (PAMAM) dendrimers-grafted magnetic-nanoparticles were synthesized and characterized, and the expected integration of more multifunctional sites of PAMAM dendrimers and rapid separation property was utilized for method development. To achieve the best extraction efficiency, several important parameters were optimized including the dosage of the adsorbent, sample pH, kind and volume of eluent , extraction time, desorption time, ionic strength . Under the optimal conditions, three phthalate esters were well enriched and simultaneously determined by high performance liquid chromatography with variable wavelength detector (VWD). Excellent linearities were observed in the range of 0.1–600 μg L −1 for DPhP and DnPP and 0.5–600 μg L −1 for DCHP, and all correlation coefficients (R 2 ) were larger than 0.997. The limits of detection (LODs, S/N = 3) were ranged from 0.025 to 0.16 μg L −1 . The spiked recoveries of PAEs in real water samples were in the range of 93.5–101.8% with satisfied relative standard deviations (RSDs) ranging from 0.9 to 4.1%. The prepared magnetic materials have shown good adsorption capability for PAEs and the developed method earned merits such as high sensitivity, simplicity, rapidness and environmental friendliness , which can be used as a robust alternative tool for monitoring PAEs in water samples.
研究领域:
环境科学
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分析化学
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PubMed
高影响因子
JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE
·
2023
·Vol. 104
·期 1
·257-265
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IF 4.1
Jie Zhao,Zi-Yu Li,Chun-Xu Yang,Ya-Ping Li,Yu-Shen Liu,Zhen Hua Hu,Xiao-Ming Pan,Xiu-Li Ma,Wei Wang,Xiao-Shuai Yang,Lu-Liang Wang
BACKGROUND Phenolic endocrine-disrupting chemicals (EDCs) are widespread and easily ingested through the food chain. They pose a serious threat to human health. Magnetic solid-phase extraction (MSPE) is an effective sample pre-treatment technology to determine traces of phenolic EDCs. RESULTS Magnetic covalent organic framework (COF) (Fe 3 O 4 @COF) nanospheres were prepared and characterized. The efficient and selective extraction of phenolic EDCs relies on a large specific surface and the inherent porosity of COFs and hydrogen bonding, π–π, and hydrophobic interactions between COF shells and phenolic EDCs. Under optimal conditions, the proposed magnetic solid-phase extraction-high-performance liquid chromatography–ultra violet (MSPE-HPLC-UV) based on the metallic covalent organic framework method for phenolic EDCs shows good linearities (0.002–6 μg mL −1 ), with R 2 of 0.995 or higher, and low limits of detection (6–1.200 ng mL −1 ). CONCLUSION Magnetic covalent organic frameworks (Fe 3 O 4 @COFs) with good MSPE performance for phenolic EDCs were synthesized by the solvothermal method. The magnetic covalent organic framework-based MSPE-HPLC-UV method was applied successfully to determine phenolic EDCs in beverage and water samples with satisfactory recoveries (90.200%–123%) and relative standard deviations (2.100%–12.100%). © 2023 Society of Chemical Industry.
研究领域:
环境科学
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分析化学
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材料科学
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DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
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2026
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IF 12.5
Sijia Zhang,YiJingdan Zhang,Yaxin Zheng,Yingying Li,Ting Wang,Xiaohong Hou
The widespread clinical use of large-volume parenteral preparations (LVP) has raised serious concerns about the migration of additives and their degradation products from plastic packaging into LVP. The simultaneous migration of multiple additives exacerbates the toxic risks of combined exposure. However, simultaneous monitoring of multiple compounds in such complex matrices remains challenging. Here, a novel magnetic solid phase extraction (MSPE) coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the enrichment and determination three plasticizers, four UV stabilizers, five antioxidants, and degradation products in both plastic packaging and LVP. The MSPE adsorbent, a newly fabricated MOF-on-MOF composite designated MIL-88 A(Fe)-500C@ZIF-8-2, was prepared via carbonization followed by surfactant-assisted growth. It exhibited a high specific surface area (1043 m 2 ·g −1 ), a hierarchical pore structure (micropores of 1.88 nm and mesopores of 3.49/13.14 nm), abundant functional groups, and excellent hydrophobicity (contact angle 137.8°), which collectively enabled efficient multisite synergistic adsorption. Key extraction parameters were optimized, yielding optimal conditions of 15 mg adsorbent, 10 min adsorption (without pH adjustment), and elution with 1.5 mL acetonitrile for 10 min. Under the optimized conditions, the method demonstrated good linearity ( r > 0.99), low detection limits (0.03–1.1 ng·g −1 for infusion bottle, 0.03–1.3 ng·g −1 for infusion bag, and 1.2–31.0 ng·L −1 for LVP), high accuracy (71.4–98.6%), and precision (RSD < 9.1%). Multiple additives were detected in actual packaging and LVP samples. Adsorption experiments revealed that the adsorption process was well described by the pseudo-second-order and Langmuir isotherm models. The adsorption behavior likely involved synergistic effects of multiple intermolecular interactions, including hydrophobic forces, π-π interactions, hydrogen bonding, and weak electrostatic interactions. This work provided a powerful analytical tool for safeguarding drug quality and a versatile material platform for the extraction of trace contaminants from complex matrices.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
IF 2.813
Shengdong Pan,Jiabin Zhang,Qian He,Xiaohong Chen,Micong Jin
In this study, novel benzenesulfonic acid groups modified magnetic microspheres (Fe 3 O 4 @SiO 2 @poly(4-VB)) were synthesized and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectrometry (FTIR), and vibrating sample magnetometer (VSM). The as-prepared Fe 3 O 4 @SiO 2 @poly(4-VB) was employed as a magnetic-phase extraction (MSPE) adsorbent for rapid determination of paraquat (PQ) and diquat (DQ) in human urine samples coupled with ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Moreover, this paper had expounded systematically the mass spectrum cracking mechanisms of PQ and DQ. And a zwitterionic functionalized SIELC Obelisc R column was employed for separation and retention of the above two polar herbicides using 50 mmol/L ammonium formate (pH = 3.7)-acetonitrile as the mobile phase. Besides, the adsorption and desorption conditions of Fe 3 O 4 @SiO 2 @poly(4-VB) toward PQ and DQ were optimized in spiking urine samples to obtain the best adsorption and desorption efficiencies. And the adsorption mechanisms of Fe 3 O 4 @SiO 2 @poly(4-VB) toward PQ and DQ referred to synergetic effect of electrostatic attraction and π-π interaction. Under the optimal conditions, the inter-day and intra-day spiking recoveries of the proposed method were in the range of 86.7–109.9% with RSDs less than 10%. The limits of detection (LODs) were obtained by spiking in blank urine samples at a series of low concentrations and were found to be 0.12 μg/L and 0.14 μg/L for PQ and DQ, respectively, which were lower than the comparing literatures. The developed analytical method was proven to be simple, rapid, sensitive, and accurate for clinical poisoning analysis.
研究领域:
分析化学
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毒理学
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临床医学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
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IF 2.8
Guohua Teng,Hezhao Bai,Chen Zhang,Jingyi Yang,Xiaoye Wang,Yu Zhu,Fei Tian
A magnetic composite (Fe 3 O 4 @SiO 2 @PNIPAM-co-NHMA) with high adsorption capacity and recoverability was developed for the enrichment and determination of flavonoids in Scutellaria Radix ( SR ). A magnetic solid-phase extraction (MSPE) technique using Fe 3 O 4 @SiO 2 @PNIPAM-co-NHMA absorbent in combination with high-performance liquid chromatography (HPLC) was developed for selectively enrichment and determination of the biologically active flavonoids in the aqueous extract of SR , including baicalein, baicalin, wogonoside and wogonin. Under the optimized experimental conditions, the magnetic adsorbent could adsorb up to 77.0 ± 0.98 % − 98.15 ± 0.15 % of four representative flavonoids from SR , with elution rates varying from 55.10 ± 0.25 % to 91.94 ± 1.85 %. The limits of detection (LOD) and limits of quantitation (LOQ) were 0.01–0.35 μg/mL and 0.03–0.98 μg/mL, respectively. In addition, it remained effective after six replicates, demonstrating its potential as a recoverable adsorbent for enriching flavonoids in traditional Chinese medicine.
研究领域:
分析化学
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药学
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纳米技术
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中医药
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PubMed
高影响因子
危险品化学品经营许可证（带存储）