Catalysts
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2025
·Vol. 15
·期 3
·197
·
IF 4
Yu Zhou,Kaixin Zheng,Yihao Zhang,Yong Zhao,Zhi Ouyang,Xu Zhang,Xianhua Liu
Black-odorous water (BOW) in urban areas poses significant risks to water safety and human health. Chemical oxygen demand (COD) is a critical parameter for the control and monitoring of BOW. However, traditional methods for COD determination are expensive, time-consuming, and involve the use of hazardous chemicals. In this study, reduced graphene oxide (rGO) and transitional metal particles (Cu, Ni) were used as working electrode materials for facile on-site determination of COD in BOW. Three composite materials (rGO/Cu, rGO/Ni, and rGO/Cu/Ni) were synthesized by one-step chemical reduction with different ratios, and their microstructure and chemical composition were characterized. Glucose solution and real water were used to evaluate the electrocatalytic performance of the different sensors. The ternary composite (rGO/Cu/Ni) screen-printed electrode sensor demonstrated excellent performance in COD analysis, with a low limit of detection (18.9 mg L−1), a broad linear detection range from 53 to 1500 mg L−1, and a 1.61% relative error for real water samples. The testing results were highly consistent with those obtained using the standard chromium sulfate method. This study offers promising prospects for the mass production of cost-effective COD electrochemical sensors, facilitating real-time, on-site monitoring of water bodies in major urban areas.
研究领域:
环境科学
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材料科学
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DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Yu Luyao,Liu Meichen,Niu Ziyi,Zhang Jiarui,Deng Yue,Zhou Xinyue,You Jiansong,Xue Hongyu,Yin Lei,Shi Meiyun
Monodisperse polyethylene glycol (PEG) derivatives offer significant advantages over conventional polydisperse PEGs for biomedical applications due to their precisely defined molecular structures. This study establishes an eco-efficient, selective, and sensitive analytical assay integrating microscale solid-phase extraction (μ-SPE) with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to investigate the cellular uptake of HO-PEG 8 -OH polymers in MCF-7 cells. The method achieved greater than 91% recovery from 20 μL lysates using M-PEG 6 -OH as the internal standard, with validated linearity (10–1000 ng/mL, R > 0.997), accuracy (relative error < ± 7.49%), and precision (RSD < 7.50%). The novelty of the assay is the harmonization of analytical performance with green analytical chemistry principles. The validated method provides a robust platform for studying monodisperse PEG derivatives while addressing growing demands for sustainable analytical technologies. Green analytical chemistry metric assessments confirmed the environmental sustainability of the method. Cellular pharmacokinetic analysis revealed time-/concentration-dependent uptake kinetics of HO-PEG 8 -OH polymers in MCF-7 cells, showing 3.2-fold accumulation between 0.5 and 48 h exposure. These findings offer important insights for PEG-based drug delivery system optimization and establish a new standard for environmentally conscious bioanalytical method development. Graphical
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PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2019
·
IF 8.355
Yue Wang,Wenchang Zhao,Xuemeng Tian,Huijia Song,Ruixia Gao,Xiaoshuang Tang,Xiaojing Zhang,Yi Hao,Yuhai Tang
Hydrophilic molecularly imprinted polymer for effective removal of pollutants from environmental water has attracted much attention due to their high selectivity and matrix compatibility. Herein, resorcinol and formaldehyde have been first proposed as the hydrophilic monomers to form water-compatible molecularly imprinted resin magnetic nanomaterials (Fe 3 O 4 -RF-MIPs) by adopting a two-step template immobilization strategy of surface molecular imprinting technique. In the synthesis process, carboxyl-modified Fe 3 O 4 nanoparticles and sulindac were adopted as carrier and template molecule, respectively. The physical and chemical properties, preparation process, and adsorption conditions of Fe 3 O 4 -RF-MIPs were investigated in detail. Fe 3 O 4 -RF-MIPs exhibit uniform morphology, high crystallinity, outstanding magnetic property, fast binding kinetics, high adsorption capacity, satisfactory selectivity, and excellent reusability. Meanwhile, combining with HPLC, Fe 3 O 4 -RF-MIPs as solid phase extraction adsorbents have been successfully applied to specifically enrich and detect sulindac in sewage water. Accordingly, Fe 3 O 4 -RF-MIPs with ordered and evenly distributed imprinted sites and excellent dispersibility in water would be potential in the field of water environmental pollution control.
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高影响因子
Polymers
·
2021
·Vol. 13
·期 17
·2935
·
IF 4.329
Yunjie Ma,Yang Ruan,Xin Gao,Hang Cui,Wei Zhang,Shaoyan Wang
A new type of economical covalent organic framework material(COF), namely resin based covalent organic framework material, was prepared by combining resin and covalent organic framework material by hydrothermal synthesis, which was based on the preparation of traditional COF material(TpBD COF). The properties of the material and covalent organic framework material were compared in the way of characterization, and the possible reaction mechanism was analyzed. The solid phase extraction separation (SPE) ability of this material for four kinds of phenolic endocrine disrupting compounds (bisphenol F, bisphenol A, octylphenol and nonylphenol) in beverage samples was investigated. The results showed that the prepared COF materials had abundant internal channels, ordered structure, large specific surface area (TpBD COF: 814.6 m2/g and resin based COF: 623.9 m2/g) and good thermal stability (pyrolysis temperature was 443 °C and 437 °C, respectively). Solid phase extraction experiments demonstrated that the two COF materials as adsorbent of solid phase extraction column had ideal adsorption separation effect and good anti-interference ability, and had strong anti-interference ability. The SPE effect was superior to the traditional solid phase extraction column. The precision RSD of this method was less than 3%. This SPE method had high recovery and could be reused (carbonated beverage: 98.18–102.18% and beverage: 98.52–101.79%), In addition, the recovery of the material did not change significantly in the 50 cycles of solid phase extraction, indicating that the material had good stability and could be reused, which could meet the requirements for the detection and analysis of trace pollutants in environmental samples. The resin based COF material prepared in this study could reduce the cost of monomer uses and provide a possibility for its industrial production. At the same time, as an efficient SPE adsorbent, it also provided a new research scheme for the enrichment of trace phenolic endocrine disruptors in beverage samples.Keywords:resin based covalent organic framework materials;phenolic endocrine disruptors;solid phase extraction;trace analysis
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
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2019
·Vol. 411
·期 18
·4073-4084
·
IF 3.286
Xia Ling,He Yuanyuan,Xiao Xiaohua,Li Gongke
Herein, a total online device based on field-assisted extraction (FAE), micro-solid-phase extraction (μ-SPE), and high-performance liquid chromatography (HPLC) was designed. Solid samples were pretreated with ultrasound-microwave synergic effects, and then the extract was cleaned up online with a monolithic column, followed by HPLC analysis. The cross-actions between ultrasound and microwave along with other extraction parameters were studied systematically. The efficiency of this online method was verified in the determination of polycyclic aromatic hydrocarbons (PAHs) in foods and tetracycline antibiotics (TCAs) in cosmetic samples. The detection limits of nine PAHs including fluorene, phenanthrene, anthracene, fluoranthene, benzo[k]fluoranthene, benz[a]anthracene, benzo[b]fluoranthene, pyrene, and benzo[a]pyrene were all within 0.075–0.30 μg/kg, as well as four TCAs including oxytetracycline, tetracycline, chlortetracycline, and doxycycline were within 0.02–0.06 μg/kg. Six PAHs were found in roast potatoes and baked fish and the recoveries were in the range of 71.5–119.7% with RSDs of 0.2–10.9% ( n = 3). The recoveries for TCAs in cosmetic samples were in the range of 75.3–118.0% with RSDs lower than 8.2% ( n = 3). Compared with those offline methods, this total online FAE-μ-SPE-HPLC method not only simplifies the operation process, but also increases the precision and accuracy. Beyond trace analytes analysis in solid and semi-solid matrixes, application of this total online analysis method can also be extended to investigate field-assisted extraction mechanisms.
Graphical abstract
研究领域:
分析化学
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环境科学
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药物分析
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PubMed
高影响因子
CHROMATOGRAPHIA
·
2024
·
IF 1.2
Han Kyoung-Moon,Woo In Suk,Park Chae Gyeong,Kim You Kyung,Yang Yoon Ji,Park Bo Reum,Choi Jang Duck,Son Kyung Hun
Preservatives can be used in natural and organic cosmetics to prevent quality deterioration during distribution and use, but the ingredients permitted are limited in the Republic of Korea. A method of simultaneous analysis was developed to monitor natural and organic cosmetics distributed online for the presence of 15 illegally used preservatives. Considering the complexities of the cosmetic matrices, an optimized sample preparation method is essential. Therefore, we developed the optimal purification method by comparing three preparation methods: QuEChERS, high-speed centrifugation, and solid-phase extraction (SPE). The SPE method, which exhibited the most favorable results in matrix reduction, was employed. To establish the SPE-ultra-high-performance liquid chromatography-diode array detection method, factors such as the mobile phase and column were optimized. The optimal separation of the 15 preservatives was observed under the following conditions: mobile phase A comprising 0.1% phosphoric acid in water with 0.5 mM sodium hexanesulfonate and a C 8 column (1.7 μm, 2.1 × 150 mm) as the stationary phase. The linear correlation coefficients were > 0.9998, and the limits of detection and quantitation ranged from 0.05 to 0.67 and 0.15 to 2.02 μg mL −1 , respectively. Using the established analytical method, illegally used preservatives were detected in products claimed to be natural and organic cosmetics sold on the market, and these findings were subsequently verified using liquid chromatography-tandem mass spectrometry. Six out of 47 samples contained phenoxyethanol and parabens. Therefore, this method will help manage the addition of illegal preservatives to natural and organic cosmetics.
研究领域:
分析化学
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化妆品科学
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高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 10
·1391-1400
·
IF 1.401
Pang Xiaomin,Bai Ligai,Lan Dandan,Guo Bin,Wang Huimin,Liu Haiyan,Ma Zhengyue
An 1-vinyl-3-hexyl imidazolium bromide ionic liquid-based monolithic column was prepared via in situ free radical polymerization, which was used as the sorbent of on-line solid phase extraction. The prepared material was characterized by scanning electron microscopy, nitrogen adsorption–desorption instrument and mercury intrusion porosimetry, respectively, and the results showed that the homemade monolith occupied relatively uniform porous structure and high-specific surface area of 212.53 m 2 g −1 . On-line solid phase extraction–high-performance liquid chromatography was performed to quantitatively analyze five steroid drugs, including betamethasone, norgestrel, halcinonide, beclomethasone dipropionate and testosterone propionate in human plasma. The determination procedure was carried out following the optimization of the mobile phase composition. Methodological validation showed that correlation coefficients of the linear regressions were in the range of 0.9989–0.9992; the values of relative standard deviation for precision were in the range of 1.39–6.15% for intra-day and 0.32–6.34% for inter-day, respectively; the values of accuracy expressed by recovery were in the range of 99.02–101.98, 93.27–102.89, 102.79–104.01, 100.04–102.61 and 100.77–102.44% for the five drugs in order, respectively; the values of relative standard deviation for repeatability calculated according to retention times and peak areas of the five drugs were in the ranges of 0.28–0.76% ( n = 5) and 0.84–2.63% ( n = 5), respectively. The results showed that the polymer monolithic column was feasible for an on-line solid phase extraction column, exhibiting good selectivity and high permeability.
研究领域:
分析化学
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药物分析
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生物化学
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高影响因子
TALANTA
·
2015
·
IF 3.545
Fengling Zhu,Jing Wang,Lijun Zhu,Lanlan Tan,Guanglin Feng,Shaomin Liu,Ya Dai,Hua Wang
In this paper, a novel dummy template molecularly imprinted polymer (DMIP) based on a vinyl-SiO 2 microspheres surface for the simultaneous selective recognition and enrichment of 18 amino acids was prepared via a surface molecular imprinting technique using theanine as a dummy template. Compared to the imprinted polymers prepared using traditional polymerization techniques, the obtained DMIPs exhibited a regular spherical shape and were relatively monodisperse. The maximal sorption capacity ( Q max ) of the resulting DMIPs for the 18 amino acids was up to 1444.3 mg g −1 . A kinetic binding study showed that the sorption capacity reached 85.40% of Q max in 25 min and sorption equilibrium at 30 min. The imprint factors of the sorbents ranged from 2.86 to 6.9 for the 18 amino acids, which indicated that the DMIP sorbents have high selectivity. An HPLC-UV method for the simultaneous determination of 18 amino acids in tobacco and tobacco smoke was developed using the DMIPs as sorbents for solid phase extraction (SPE) in the sample pretreatment procedure. Under the optimum experimental conditions, the materials had enrichment factors of up to 200 for the amino acids, and the recoveries of the 18 amino acids in tobacco smoke were in the range from 79% to 104% with relative standard deviations of less than 7.4%. It indicated that the obtained DMIP sorbents could specifically recognize the amino acids from complicated samples.
研究领域:
分析化学
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食品科学
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PubMed
高影响因子
Foods
·
2022
·Vol. 11
·期 3
·386
·
IF 5.561
Ying Xu,Xuan Yu,Jiaqi Gui,Yiqun Wan,Jinping Chen,Ting Tan,Fan Liu,Lan Guo
A rapid and effective ultra-high performance liquid chromatography (UHPLC) method was developed for the determination of five anthraquinones (emodin, physcion, aloe-emodin, rhein, and chrysophanol) inPolygonum multiflorum. The target compounds were ultrasonically extracted with 70% methanol, followed by dispersive solid-phase extraction (d-SPE) with HC-C18 and desorption with acetonitrile. The five anthraquinones were separated on an ACQUITY UPLC®HSS T3 column (2.1 × 100 mm, 1.8 μm) and detected by a photodiode array detector (PDA) at 254 nm. Under the optimized conditions, linear relationships were achieved in the range of 0.3~100 mg/L for emodin, 0.3~40 mg/L for physcion, 0.1~20 mg/L for aloe-emodin, and 0.05~20 mg/L for rhein and chrysophanol. The limits of detection of the five analytes ranged from 0.01 to 0.08 mg/L, and the recoveries were within the range of 82.8~118.4% with an RSD (n= 6) of 1.0~10.3%. The intra-day and inter-day precision (n= 5) of the five targets were in the range of 1.0~1.8% and 3.0~3.1%, respectively. Furthermore, this method was applied to analyses ofPolygonum multiflorumsamples collected from different regions in China with satisfactory results. All the results indicated that this method is suitable for the detection of five anthraquinones inPolygonum multiflorum.Keywords:anthraquinones;Polygonum multiflorum;d-SPE;UHPLC
研究领域:
分析化学
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中药学
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PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2023
·Vol. 37
·期 13
·e9518
·
IF 2
Lihua Qu,Xiaoyu Qi,Li Zhao,Yu Zhang,Ronghua Zhuge,Zhihui Hao,Congmin Liu
Rationale The residues of fipronil and its metabolites in chicken eggs pose a threat to human health, so regular monitoring is necessary. However, the pretreatments of the existing detection methods are complex and time-consuming. A simple and streamlined pretreatment method is needed to improve the detection efficiency. Method A rapid, efficient, and facile approach employing the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method with online solid-phase extraction liquid chromatography tandem Q Exactive Orbitrap high-resolution mass spectrometry (online-SPE-LC-HRMS) was established and evaluated for the determination of fipronil, fipronil-desulfinyl, fipronil-sulfone, and fipronil-sulfide in chicken eggs. An improved sample preparation technique combining QuEChERS and online-SPE was developed. Negative targeted ion fragmentation scanning and targeted-selected ion monitoring of HRMS were adopted to identify and quantify the target analytes. Results The proposed pretreatment method took a few steps in <13 min to achieve excellent recoveries and negligible interference. High selectivity was acquired with the adoption of Q/Orbitrap HRMS. The limit of quantification (LOQ) of the analytes was 2.5 μg kg −1 , meeting the detection requirements of the maximum residue level enacted by the Codex Alimentarius Commission, Japan, and the United States for the sum of fipronil and its metabolites. Extraction recoveries at three spiked concentration levels were within 84.56% to 93.84%, with relative standard deviation ≤5.87%. Conclusion The established method is efficient and easy to operate and displays satisfactory LOQs, recoveries, accuracy, and precision. This approach serves as a reference method for monitoring eggs while providing potential solutions for fipronil determination in more complicated matrices.
研究领域:
食品安全
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分析化学
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毒理学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Xiaoya Fu,Xia Wang,Zhining Xia,Yike Huang
To ensure drug safety, the quality monitoring of genotoxic impurities (GTIs) which have very trace content in medicine is important. Therefore, it should be established an efficient sample pretreatment method to extract GTIs to achieve specific enrichment. In this work, dummy template molecular imprinting technology (DMIT) was used as dummy template molecule (DTM) to substitute for the target molecule (TM) for established the pretreatment of the sample containing aromatic amine GTIs. A novel strategy for screening out DTM by calculation of computer simulation is established, where the binding energy between the template and functional monomer has the relatively lowest value (-9.60 kcal/mol). Then dummy template molecular imprinted polymer (DMIP) was prepared by bulk polymerization according to the molar ratio of template molecule-functional monomer-crosslinker = 1:4:8, the prepared DMIP exhibited the highest adsorption ( Q = 8.6 mg/g) and good blotting effect (IF = 1.3) and can simultaneously adsorb three aromatic amine GTIs. The optimal adsorption conditions were obtained by conditional optimization of solid phase extraction (SPE). The solution of pH 7 was chosen as the loading condition, and methanol/acetic acid (90:10, v/v) was chosen as the elution condition. Finally, we determined 2, 6-dichloroaniline in diclofenac sodium at a 5 ppm level and p-toluidine as the TMs in torasemide sample at 10 ppm by using DMIT-based solid phase extraction and analysis by HPLC, it satisfied the quality control of GTIs in pharmaceutics. DMIT by this strategy has great potential in the sample preparation of GTIs.
研究领域:
药学
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分析化学
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药物安全性评价
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Rujia Shen,Lijin Huang,Ruiqi Liu,Qin Shuai
In this work, hierarchical porous covalent organic frameworks (HP-COFs) foam, named as HP-TpBD, was prepared by using 1,3,5-trimethylphloroglucinol (Tp) and benzidine (BD) as building blocks under the assistant of NaCl template. Its potential application as the sorbent for solid phase extraction (SPE) of sulfonamides (SAs) in meat products were explored by coupling with high performance liquid chromatography-mass spectrum (HPLC-MS) analysis. The key factors affecting extraction efficiency were well studied. Under the optimum conditions, the proposed method exhibited high preconcentration factors of 100, low limit of detection (0.10-0.23 μg/kg), and wide linear ranges (0.5-200 μg/kg). In addition, the determination of SAs in real samples were realized with satisfactory recoveries (82.8-119.9%), demonstrating the applicability of the proposed method. The easy operation, superior extraction affinity and good recycle performance demonstrated the resulting HP-COF foam is a promising adsorbent for the preconcentration of trace organic compounds from complex matrix.
研究领域:
分析化学
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食品科学
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材料科学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）