MOLECULES
·
2024
·Vol. 29
·期 10
·2311
·
IF 4.2
Ling Yu,Aiqing Xia,Yongchao Hao,Weitao Li,Xu He,Cuijuan Xing,Zan Shang,Yiwei Zhang
Pyrethroid pesticides (PYRs) have found widespread application in agriculture for the protection of fruit and vegetable crops. Nonetheless, excessive usage or improper application may allow the residues to exceed the safe limits and pose a threat to consumer safety. Thus, there is an urgent need to develop efficient technologies for the elimination or trace detection of PYRs from vegetables. Here, a simple and efficient magnetic solid-phase extraction (MSPE) strategy was developed for the simultaneous purification and enrichment of five PYRs in vegetables, employing the magnetic covalent organic framework nanomaterial COF-SiO2@Fe3O4as an adsorbent. COF-SiO2@Fe3O4was prepared by a straightforward solvothermal method, using Fe3O4as a magnetic core and benzidine and 3,3,5,5-tetraaldehyde biphenyl as the two building units. COF-SiO2@Fe3O4could effectively capture the targeted PYRs by virtue of its abundant π-electron system and hydroxyl groups. The impact of various experimental parameters on the extraction efficiency was investigated to optimize the MSPE conditions, including the adsorbent amount, extraction time, elution solvent type and elution time. Subsequently, method validation was conducted under the optimal conditions in conjunction with gas chromatography–mass spectrometry (GC-MS). Within the range of 5.00–100 μg·kg−1(1.00–100 μg·kg−1for bifenthrin and 2.5–100 μg·kg−1for fenpropathrin), the five PYRs exhibited a strong linear relationship, with determination coefficients ranging from 0.9990 to 0.9997. The limits of detection (LODs) were 0.3–1.5 μg·kg−1, and the limits of quantification (LOQs) were 0.9–4.5 μg·kg−1. The recoveries were 80.2–116.7% with relative standard deviations (RSDs) below 7.0%. Finally, COF-SiO2@Fe3O4, NH2-SiO2@Fe3O4and Fe3O4were compared as MSPE adsorbents for PYRs. The results indicated that COF-SiO2@Fe3O4was an efficient and rapid selective adsorbent for PYRs. This method holds promise for the determination of PYRs in real samples.
研究领域:
分析化学
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环境科学
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食品科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Yifu Jiang,Le Lang,Jingwen Zhang,Yining Ji,Chenglong Zhang,Ruiqin Yang,Xuwen Li
This study combined the structural characteristics of amanita peptide toxins to prepare a Fe 3 O 4 /P4VPBA/PPy/GO composite material as a magnetic solid-phase extraction adsorbent. The experimental results indicated that this adsorbent showed excellent selectivity for the extraction of amatoxins and phallotoxins from mushroom samples. Compared with traditional dispersive solid-phase extraction, this adsorbent enables rapid separation in the enrichment and elution recovery stages through the application of a magnetic field . Simultaneously, the study optimized the conditions for ultraperformance liquid chromatography–mass spectrometry (UPLC–MS/MS), ensuring both separation efficiency and accuracy while reducing the analysis time. The researchers established the MSPE–UPLC–MS/MS method for the determination of amanita peptide toxins in wild mushrooms. This method not only simplified and expedited the sample pretreatment process but also achieved qualitative and quantitative analyses in a short period, thus demonstrating high detection sensitivity and outstanding recovery rates. Furthermore, the developed method was successfully applied to analyze toxic mushrooms discovered in Nanjing, China. The potential for extensive utilization of this method is highlighted in the field of food analysis and detection.
研究领域:
分析化学
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食品科学
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毒理学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Yi-Xin Zhong,Chun-Ying Xu,Yi-Fan Cao,Hong-Liang Li,Cheng-Xiong Yang
Aromatic amines (AAs) are a typical class of carcinogenic contaminants frequently present in food packaging materials. Considering the huge consumption of tea beverages in our daily life and the frequently usage of packaging materials in tea beverages, establishment of sensitive and selective method to detect polar and trace AAs in tea beverages is urgently needed. Herein, a sulfonamide-functionalized magnetic microporous organic network (MMON-SO 2 NH 2 ) was synthesized for the efficient magnetic solid-phase extraction (MSPE) of AAs from tea beverages through the pre-designed electrostatic attraction, π-π, hydrophobic, and hydrogen bonding interactions. MMON-SO 2 NH 2 demonstrated large surface area (304.4 m 2 g -1 ), rapid magnetic responsiveness (38.3 emu g -1 , < 15 s), and good stability and reusability (> 8 times), being an ideal magnetic adsorbent for AAs. The established MMON-SO 2 NH 2 −MSPE-HPLC-UV method gave wide linear ranges (1–1000 µg L -1 ), low limits of detection (0.3–1.0 µg L -1 ) and limits of quantitation (1.0–3.0 µg L -1 ), large enrichment factors (80.3–85.6), and good anti-interference ability. Satisfactory recoveries were obtained, which demonstrated the potential of MMON-SO 2 NH 2 for efficient enrichment of trace AAs in complex samples and uncovered the promising of sulfonamide-functionalized magnetic adsorbent in sample pretreatment.
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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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2020
·Vol. 413
·期 1
·215-223
·
IF 3.637
Li Na,Zhao Tengwen,Du Li,Zhang Ziyang,Nian Qixun,Wang Manman
A graphitic carbon nitride (g-C 3 N 4 /Fe 3 O 4 )–based magnetic solid-phase extraction (MSPE) approach was established for fast and simple analysis of estrogens in milk powders. The composites were characterized by X-ray diffractometer, scanning electron microscope, and Brunauer-Emmett-Teller surface area and pore size distribution analyzer. Compared with the bulk g-C 3 N 4 , g-C 3 N 4 /Fe 3 O 4 gave a narrower distribution of mesopores and provided an enhanced surface area from 77.1 to 113.7 m 2 /g. Polar analytes of estrogens were selected as model compounds and the extraction of four estrogens was achieved in n-hexane using 15 mg of adsorbent within only 2 min. Possible extraction mechanism of g-C 3 N 4 /Fe 3 O 4 for these estrogens was explored in terms of the polarity of the analytes and the adsorption performance of the adsorbent. The hydrophobicity and the hydrogen-bond interaction between the estrogens and g-C 3 N 4 were responsible for the efficient adsorption. Combined with HPLC, MSPE with the prepared adsorbent gave the enhancement factors of 20 to 24 and the linear ranges of 2–200 μg/kg for 17 β -estradiol and 17 α -ethinylestradiol, 1.5–150 μg/kg for estrone, and 3–300 μg/kg for hexestrol. The detection limits and quantification limits for the estrogens in milk powders were 0.5–0.9 μg/kg and 1.5–3.0 μg/kg, respectively. The recoveries varied from 75.1 to 97.2%, with the intra-day and inter-day precisions ≤ 14.2%. Furthermore, the enrichment of the analytes and the clean-up of fat and protein interferences were achieved simultaneously with one-step g-C 3 N 4 -based MSPE. The present method was convenient, fast, and sensitive, and therefore could be successfully applied for the determination of estrogens in milk powders.
Graphical abstract
研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2020
·Vol. 44
·期 19
·7727-7739
·
IF 3.288
Hui Wang,Shaowei Yan,Bo Qu,He Liu,Jie Ding,Nanqi Ren
A rapid and efficient magnetic solid phase extraction (MSPE) method, based on Fe3O4@β-cyclodextrin–lipid bilayer nanocomposites (Fe3O4@β-CD–LB), was built. The MSPE method coupled with GC-QTOF-MS has been designed for the trace detection of nine organochlorine pesticides (OCPs) in soil samples. The Fe3O4@β-CD–LB was successfully synthesized and characterized by vibrating sample magnetometry, Fourier transform infrared spectrometry, transmission electron microscopy, field emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. In this experiment, the OCPs in the soil samples were firstly extracted with n-hexane/dichloromethane (v/v 1 : 1) at high pressure and temperature, and then subjected to MSPE for adsorption and purification. Considering the synergy effect between host–guest inclusion complexation and hydrophobic interaction in the adsorption mechanism, the bi-functionalized magnetic nanocomposites exhibited excellent adsorption properties for the OCPs and natural resistance to interference by macromolecules. Under the optimum experimental conditions, the method showed wide linear ranges with low limits of detection (4.5 to 34 pg g−1). The results showed that the mean recoveries of the OCPs in the soil samples were 78–107% with 3.0–6.1% intra-day relative standard deviation (RSD) and 3.5–6.9% inter-day RSD. The method has been applied for the determination of the OCPs in actual samples, and ΣOCPs ranged between 0 and 2.3 ng g−1 in seven soil samples.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
Analytical Methods
·
2017
·Vol. 9
·期 39
·5763-5768
·
IF 1.9
Yan Pan,Zhifen Deng,Yanlong Chen,Wenfen Zhang,Zhicong Yang,Wenjie Zhao,Shusheng Zhang
In this study, a sensitive and practical method for the determination of benzo[a]pyrene (BaP) in smoked foods with HPLC-FLD was developed. In order to improve the detection limit of HPLC-FLD, we prepared magnetic nanoparticles with monomers of 4,4′-bipyridine and cyanuric chloride (Fe3O4@TCLN) used as a sorbent in magnetic solid-phase extraction (MSPE) to extract trace BaP from the samples. The recovery was 94.74% for BaP, and the limit of detection (LOD) and limit of quantification (LOQ) were 0.09 μg kg−1 and 0.28 μg kg−1, respectively. As a result of BaP analysis from real smoked foods, the average BaP content was 5.68 μg kg−1 and the highest content of BaP was 6.12 μg kg−1. The developed method could be potentially used for the determination of BaP in food safety analysis and monitoring.
研究领域:
食品安全
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分析化学
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产品关联
DOI
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2021
·
IF 1.312
Limin Ren,Yingying Huang,Bingshan Zhao,Lanying Xu,Tao Long
A fast, simple, and efficient sample pretreatment technique based on magnetic dodecyl functionalization of magnetic ferrite microspheres has been developed for the extraction and pre-concentration of phthalate esters from environmental water prior to high-performance liquid chromatography analysis. The magnetic composite microspheres were prepared using Fe3O4 microspheres as magnetic core and silica as a shell with the surface-modified with C12 material. The structure of the prepared microspheres was characterized by Fourier transform infrared spectrometry, scanning electron microscopy, and vibrating sample magnetometry. Three kinds of phthalate esters were selected as model compounds to optimize the main parameters that affect extraction efficiencies, such as adsorbent dosage, sample volume, salt addition, extraction time, pH of sample solution, desorption time, eluent type, and volume. Under the optimal conditions, limits of detection (LODs) of 0.025–0.107 ng mL−1 and limits of quantification (LOQs) of 0.083–0.357 ng mL−1 were achieved. The developed method was applied for the detection of the three PAEs in a spiked sample of river water, and satisfactory recoveries in the range of 76.3–98.9% were obtained with good repeatability (RSD < 4.7%). The entire analysis process can be completed in about 30 min.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Shu-Hui Huo,Hai-Yan An,Jing Yu,Xue-Feng Mao,Zhe Zhang,Lei Bai,Yan-Feng Huang,Peng-Xin Zhou
In this study, we report a facile, environmental friendly fabrication of a type of magnetic metal-organic framework (MOF) MIL-100 that can be used for magnetic solid-phase extraction (MSPE). The magnetic MOF composites were fabricated using in situ calcination method. The as-synthesized materials exhibited both high porosity and magnetic characteristics. They used for the MSPE of polycyclic aromatic hydrocarbons (PAHs) from water samples. Such MOF-based magnetic solid-phase extraction in combination with gas chromatography equipped with a flame ionization detector (GC-FID), exhibited wide linearity (0.02–250 μ g L −1 ), low detection limits (4.6-8.9 ng L −1 ), and high enrichment factors (452–907) for PAHs. The relative standard deviations (RSDs) for intra- and inter-day extractions of PAHs were ranging from 1.7% to 9.8% and 3.8% to 9.2%, respectively. The recoveries for spiked PAHs (1 μ g L −1 ) in water samples were in the range of 88.5% to 106.6%. The results showed that the special anion-π orbital (electron donor-acceptor) interaction and π-π stacking between magnetic MIL-100 and PAHs play an important role in the adsorption of PAHs.
研究领域:
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Qian Wen,Yuzhi Wang,Kaijia Xu,Na Li,Hongmei Zhang,Qin Yang,Yigang Zhou
Amino functional dicationic ionic liquid (AFDCIL) was prepared and then coated on the surface of magnetic graphene oxide (GO) as a new magnetic adsorbent (Fe@GO@AFDCIL) for the magnetic solid-phase extraction (MSPE) of protein. The Fe@GO@AFDCIL composite was characterized by vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA), field emission scanning electron microscopy (FESEM) and zeta-potential nanoparticles . The bovine hemoglobin (BHb) was used as the analyte, and the extraction performance of Fe@GO@AFDCIL was investigated in the MSPE procedure. The concentration of BHb in samples was determined by a UV–vis spectrophotometer. A comparative investigation of Fe@GO@AFDCIL composite and traditional IL-coated Fe@GO composites (Fe@GO@IL) exhibited the benefits of Fe@GO@AFDCIL. The adsorbed BHb could be eluted from the Fe@GO@AFDCIL by 4% sodium dodecyl sulfate (SDS) solution. The Fe@GO@AFDCIL exhibited favorable stability which could be reused at least 15 times. Under the optimized condition, the real samples were investigated, which demonstrated that the Fe@GO@AFDCIL was able to be applied in extracting bovine hemoglobin (BHb) from real biological samples.
研究领域:
分析化学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 7
·2088
·
IF 4.927
Xue-Li Liu,Yong-Hui Wang,Shu-Yue Ren,Shuang Li,Yu Wang,Dian-Peng Han,Kang Qin,Yuan Peng,Tie Han,Zhi-Xian Gao,Jian-Zhong Cui,Huan-Ying Zhou
The efficient capture of multi-pollutant residues in food is vital for food safety monitoring. In this study, in-situ-fabricated magnetic MIL-53(Al) metal organic frameworks (MOFs), with good magnetic responsiveness, were synthesized and applied for the magnetic solid-phase extraction (MSPE) of chloramphenicol, bisphenol A, estradiol, and diethylstilbestrol. Terephthalic acid (H2BDC) organic ligands were pre-coupled on the surface of amino-Fe3O4composites (H2BDC@Fe3O4). Fe3O4@MIL-53(Al) MOF was fabricated by in-situ hydrothermal polymerization of H2BDC, Al (NO3)3, and H2BDC@Fe3O4. This approach highly increased the stability of the material. The magnetic Fe3O4@MIL-53(Al) MOF-based MSPE was combined with high-performance liquid chromatography-photo diode array detection, to establish a novel sensitive method for analyzing multi-pollutant residues in milk. This method showed good linear correlations, in the range of 0.05–5.00 μg/mL, with good reproducibility. The limit of detection was 0.004–0.108 μg/mL. The presented method was verified using a milk sample, spiked with four pollutants, which enabled high-throughput detection and the accuracies of 88.17–107.58% confirmed its applicability, in real sample analysis.Keywords:magnetic metal organic framework (MMOFs);magnetic solid-phase extraction (MSPE);multi-pollutants;high-performance liquid chromatography (HPLC)
研究领域:
食品安全
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Tao Ning,Siyuan Di,Zihan Li,Haokun Zhang,Zhangdi Peng,Hucheng Yang,Pin Chen,Yue Bao,Yixin Zhai,Shukui Zhu
A novel porphyrin-based magnetic covalent organic framework (PCOF) was first reported by using a facile synthetic procedure. The Fe 3 O 4 @NH 2 @PCOF nanospheres were utilized to effectively extract personal care products in a wide polarity range (log K ow values from 1.96 to 7.60). The successful magnetic solid-phase extraction (MSPE) of target analytes could be ascribed to the sufficient oxygen-, nitrogen- and phenyl-containing functional groups of the COF layer, which are demonstrated to be of good compatibility with pollutants exhibiting different polarities by using molecular dynamics simulations , independent gradient model analysis and various characterizations. The MSPE extraction efficiency was enhanced by optimizing key parameters. The findings indicated that the method had a wide linearity range (1–500 ng mL −1 for parabens and UV filters) and low detection limits (0.4–0.9 ng mL −1 for parabens and 0.2–0.6 ng mL −1 for UV filters). The accuracy was reflected by recoveries ranging from 74% to 114%. Satisfactory intra- and inter-day precisions from 3.0% to 9.8% and 0.5%–9.1% were obtained. Overall, the proposed MSPE-HPLC method is accurate and reliable for identifying parabens as well as UV filters in wastewater and swimming pool water. The potential of the method for evaluating human exposure risk was unfolded.
研究领域:
环境科学
·
材料科学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2016
·
IF 1.088
Shuangqiao Ju,Mousheng Liu,Yaling Yang
Magnetic solid-phase extraction was used for the preconcentration of cadmium, lead, and cobalt in Moringa Oleifera with determination by flame atomic absorption spectrometry. Fe3O4 nanoparticles were modified by oleic acid to form the sorbent for magnetic solid-phase extraction. The modified sorbent was characterized by transmission electron microscopy, infrared spectroscopy, and X-ray diffraction. The preconcentration was optimized for the mass of nanoparticles, pH, adsorption time, the presence of coexisting ions, solution volume, eluent, and reuse. The optimized limits of detection were 0.09, 0.26, and 0.54 µg/L for Cd(II), Pb(II), and Co(II) with relative standard deviations below 4.3%. The method was employed for the analysis of Moringa oleifera and recoveries between 90.0 and 102.0% were obtained.
研究领域:
分析化学
·
环境毒理学
·
植物营养学
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食品安全
·
重金属检测
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）