JOURNAL OF CHROMATOGRAPHY A
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2013
·
IF 4.612
Beibei Chen,Yunlin Huang,Man He,Bin Hu
A new method of hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for simultaneous analysis of various environmental estrogens. Taking eight environmental estrogens (17β-estradiol (E2), estrone (E1), estriol (E3), 17α-ethynylestradiol (EE), diethylstilbestrol (DES), dienestrol (DIS), bisphenol-A (BPA) and 4-t-octylphenol (OP)) as the target analytes, the factors affecting HF-LLLME-HPLC-UV were investigated in detail. Under the optimized experimental conditions, the extraction efficiency of HF-LLLME for eight target estrogens was in the range of 13.9–62.8%, and the enrichment factor was 88–376-fold. The limits of detection (LODs) of the proposed method for eight target estrogens of ES, BPA, E2, EE, E1, DES, DIS and OP were 0.11, 0.055, 0.66, 0.55, 0.51, 0.20, 0.11 and 1.46 ng/mL, respectively, which are lower than that obtained by some other sample pretreatment methods followed by HPLC-UV analysis. The relative standard deviations of the method (RSDs, c E3, BPA, DIS =5 ng/mL, c E1, E2, EE, OP = 40 ng/mL, c DES = 15 ng/mL, n = 7) are in the range of 5.5–8.4%. The developed method was applied for the determination of environmental estrogens in environmental and biological samples (sediment and fish), and none of the eight target estrogens was detected. The recoveries for the spiking samples with low, medium and high spiking levels were in the range of 73.2–117.5%. The proposed method has been demonstrated to be suitable for simultaneous determination of multiple environmental estrogens with high sensitivity, high enrichment factors, good sample clean-up ability and no derivatization required.
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JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 36
·期 16
·2691-2697
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IF 2.591
Haiyan Zhao,Zilin Chen
An electrophoretically mediated microanalysis method with partial filling technique was developed for screening aromatase inhibitors in traditional Chinese medicine. The in-capillary enzymatic reaction was performed in 20 mM sodium phosphate buffer (pH 7.4), and sodium phosphate buffer (20 mM, pH 8.0) was used as a background electrolyte. A long plug of coenzyme reduced β-nicotinamide adenine dinucleotide 2′-phosphate hydrate dissolved in the reaction buffer was hydrodynamically injected into a fused silica capillary followed by the injection of reaction buffer, enzyme, and substrate solution. The reaction was initiated with a voltage of 5 kV applied to the capillary for 40 s. The voltage was turned off for 20 min to increase the product amount and again turned on at a constant voltage of 20 kV to separate all the components. Direct detection was performed at 260 nm. The enzyme activity was directly assayed by measuring the peak area of the produced β-nicotinamide adenine dinucleotide phosphate and the decreased peak area indicated the aromatase inhibition. Using the Lineweaver–Burk equation, the Michaelis–Menten constant was calculated to be 50 ± 4.5 nM. The method was applied to the screening of aromatase inhibitors from 15 natural products. Seven compounds were found to have potent AR inhibitory activity.
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APPLIED SURFACE SCIENCE
·
2015
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IF 2.711
Yuan Tan,Lijing Jing,Yonghong Ding,Tianxin Wei
This work aimed to prepare a novel double-layer structure molecularly imprinted polymer film (MIF) on the surface plasmon resonance (SPR) sensor chips for detection of testosterone in aqueous media. The film was synthesized by in-situ UV photo polymerization. Firstly, the modification of gold surface of SPR chip was performed by 1-dodecanethiol. Then double-layer MIF was generated on the 1-dodecanethiol modified gold surface. The non-modified and imprinted surfaces were characterized by atomic force microscopy (AFM), fourier transform infrared (FTIR) spectroscopy and contact angle measurements. Analysis of SPR spectroscopy showed that the imprinted sensing film displayed good selectivity for testosterone compared to other analogues and the non-imprinted polymer film (NIF). Within the concentrations range of 1 × 10 −12 –1 × 10 −8 mol/L, the coupling angle changes of SPR were linear with the negative logarithm of testosterone concentrations ( R 2 = 0.993). Based on a signal/noise ratio of three, the detection limit was estimated to be 10 −12 mol/L. Finally, the developed MIF was successfully applied to the seawater detection of testosterone. The results in the experiments suggested that a combination of SPR sensing with MIF was a promising alternative method for detection of testosterone in aqueous media.
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JOURNAL OF CHROMATOGRAPHY A
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2017
·
IF 3.981
Juanjuan Wu,Ruiyang Ma,Lin Hao,Chun Wang,Qiuhua Wu,Zhi Wang
A hypercrosslinked organic polymer material (named as PPTPA) was prepared by a simple one-step self-polycondensation of triphenylamine. A series of characterization experiments, including N 2 adsorption, scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectra, and thermogravimetric analysis, were carried out to evaluate the morphology, structure and other intrinsic properties of the PPTPA. To investigate its adsorption performance, the PPTPA was used as the solid-phase extraction adsorbent for the extraction of phenylurea herbicides from water, milk and tomato juice samples followed by high-performance liquid chromatographic analysis. Under optimum conditions, good linearity for the analytes was observed in the range of 0.05–40.0 ng mL −1 , 0.1-40.0 ng mL −1 and 0.5–40.0 ng mL −1 for water, milk and tomato juice samples, respectively. The established method also showed low limits of detection (S/N = 3) in the range of 0.008–0.01 ng mL −1 , 0.01–0.03 ng mL −1 and 0.05–0.1 ng mL −1 for water, milk and tomato juice samples, respectively. The possible adsorption mechanism of the PPTPA towards the analytes was investigated, and the results demonstrated that the hydrogen bonding was the main interaction force between the PPTPA and the analytes. It suggests that the PPTPA can serve as a promisingadsorbent for the efficient pre-enrichment of organic compounds with more hydrogen-bonding donor sites.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Hailong Peng,Mei Luo,Hua Xiong,Ningxiang Yu,Fangjian Ning,Jieping Fan,Zheling Zeng,Jinhua Li,Lingxin Chen
Photonic-magnetic responsive molecularly imprinted microspheres (PM-MIMs) were prepared by seed polymerization, through suitable functionalization of magnetic nanoparticles for further coating with photoresponsive functional monomer and imprinted layers, and then were successfully applied to the fast and selective extraction of 17β-estradiol (17β-E 2 ) from real samples. The PM-MIMs possessed a sandwich micro-spherical structure containing Fe 3 O 4 core, SiO 2 middle layer, and MIPs shell with thickness of 25 nm. The PM-MIMs displayed excellent photoresponsive properties and could be rapidly separated from solutions under an external magnet. The PM-MIMs had specific affinity towards 17β-E 2 with high adsorption capacity ( Q max = 0.84 mg g −1 ) and fast binding kinetics ( K d = 26.08 mg L −1 ). The PM-MIMs proved to be an ideal photoswitch with the ability of reversible uptake and release of 17β-E 2 upon alternate 365 and 440 nm irradiation: 45.0% of 17β-E 2 released from the PM-MIMs upon 365 nm irradiation, and 94.0% of the released 17β-E 2 was rebound to the PM-MIMs at 440 nm. Accordingly, the PM-MIMs were applied for fast separation and extraction of 17β-E 2 followed by HPLC-UV determination, presenting the low limit of detection (LOD, S/N = 3) and quantification (LOQ, S/N = 10) of 0.18 and 0.62 μmol L −1 , respectively. The high recoveries for spiked milk powder and drinking water samples were in the range of 97.5–113.0% with relative standard deviations less than 4.4%. This study reasonably combined photonic response, magnetic separation and surface imprinting, which endowed the PM-MIMs with significant advantages of high adsorption capacity and fast binding kinetics, convenient separation and recycled use, and simple rapid eco-benign adsorption/elution processes for template molecules. Thus, the PM-MIMs based method may be a simple, rapid, convenient, cost-effective and environmentally-friendly way for simultaneous separation, enrichment and detection of trace 17β-E 2 in complicated matrices.
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APPLIED BIOCHEMISTRY AND BIOTECHNOLOGY
·
2016
·Vol. 182
·期 2
·482-494
·
IF 1.606
Bai Yin,Zhou Wen-Di,Mu Xian-Min,Zhang Qian,Yu Chen,Di Bin,Su Meng-Xiang
Human 17β-hydroxysteroid dehydrogenase type 1 (17β-HSD1), a potential target in breast cancer prevention and therapy, was extracted from human placenta and immobilized on nonporous silica (∼5 μm) with a covalent method for the first time. The optimum initial enzyme concentration and immobilization time during the immobilization process were 0.42 mg mL −1 and 12 h, repectively. The binding was confirmed by scanning electron microscope (SEM) and infrared spectroscopy (FT-IR). It could improve the pH, thermal and storage stability compared to free enzyme. Moreover, the immobilized enzyme could be reused at least four times. A screening method based on it coupled with liquid chromatography–time-of-flight mass spectrometer (LC-TOF/MS) was established, and the half-maximal inhibitory concentration (IC 50) of apigenin for the immobilized enzyme was 291 nM. Subsequently, 10 natural products were evaluated leading to inhibition of the activity of 17β-HSD1 at the concentration of 25 μM, and six of them inhibit the activity over 50%.
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BIOSENSORS & BIOELECTRONICS
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2017
·
IF 7.78
Mai Luo,Yifan Hua,Yiran Liang,Jiajun Han,Donghui Liu,Wenting Zhao,Peng Wang
A novel functionalized carbon dot has been synthesized by covalently linking β-cyclodextrin to the surface of N, S codoped carbon dots (β-CD-CDs). The characterization was confirmed by transmission electron microscopy , X-ray photoelectron spectroscopy, infrared spectra, ultraviolet-visible, and fluorescence emission spectra. On the basis of this carbon dot and (ferrocenylmethyl) trimethylammonium iodide (Fc + ), a photo-induced electron transfer (PET) fluorescent probe system was developed to determine the concentration of testosterone in water and identify testosterone in cell by fluorescence imaging as a visible biomarker. Under the optimum condition, the fluorescent intensity of the probe system linearly responded to the concentration of testosterone from 0 μM to 280 μM and the limit of detection was 0.51 μM. This probe system also performed well at determining testosterone in groundwater with average recoveries of testosterone ranging from 96% to 107% at spiking levels of 0.5–100 μM, and the relative standard deviation remained below 13%, which provided a reliable, rapid and easy method to determine testosterone in environmental water. Furthermore, the low cytotoxicity, high anti-interference ability, and excellent biocompatibility of β-CD-CDs made this probe system successfully used in cell fluorescence imaging to monitor levels of testosterone in the cytoplasm of cells with a promising application value in medical research.
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2017
·Vol. 24
·期 8
·7042-7050
·
IF 2.741
Zhang Dai,Zhou Lifang,Lei Yajing,Zhou Zhan,Zhou Jie,Chen Shuqing
Diethylstilbestrol (DES) is used as a kind of animal feed additive and affects people’s health through the food chain. The purpose of this study is to detect the residue level of DES in 576 human urine samples directly. DES-BSA was used to immunize Balb/c mice. The monoclonal antibody was produced by hybridoma that was screened through cell fusion techniques. Finally, we developed the indirect competitive ELISA method to analyze 576 human urine samples from Zhejiang Province, China. The IC 50 of this method was 3.33 ng/mL. The LOD and LOQ were 0.16 and 0.54 ng/mL. Linear range of the standard curve was from LOD to 12.50 ng/mL. There was no cross-reactivity with two kinds of estrogens and two structural analogs with DES. Five hundred seventy-six urine samples were analyzed by the indirect competitive ELISA method, and the detection rate was 98.78%. The mean concentration and geometric mean were 4.70 and 3.50 ng/mL. The indirect competitive ELISA method based on monoclonal antibody was sensitive and reliable for the detection of DES in human urine samples. The results warned us to pay more attention to human health and food safety.
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JOURNAL OF ENVIRONMENTAL MANAGEMENT
·
2025
·
IF 8.4
Xiaoman He,Dongyang Liu,Yue Teng,Hanzhi Wang,Qirui Wu,Wei Wang,Jingzheng Ren,Liandong Zhu
The co-culture system of Chlorella sorokiniana and Aspergillus oryzae has demonstrated exceptional tolerance and efficiency in the removal of pollutants from swine manure. This study evaluates the ability of the co-culture system to remove Zn(II) and estrone, while assessing the impact of these pollutants on the system's overall functionality. Results indicated that co-cultivation achieved higher biomass accumulation, peaking at 0.88 g/L after 96 h. Increasing estrone exposure concentration reduced photosynthetic activity and chlorophyll content, whereas Zn(II) exposure initially enhanced and later inhibited chlorophyll synthesis. Co-cultivation secreted extracellular polymeric substances, including protein-like and humus-like substances, to alleviate environmental stress and form algal-fungal community. After 96 h of cultivation, the removal efficiencies reached 86.44% for 1.5 mg/L Zn(II) and 84.55% for 20 mg/L estrone. The Quantitative Structure Activity Relationship model revealed a reduction in the ecotoxicity of estrone intermediate products to varying degrees. Metabolomics analysis showed that exposure to estrone and Zn(II) significantly boosted the production of Gibberellic acid, Indole-3-acetic acid, and Zeatin riboside in Chlorella sorokiniana , while reducing Abscisic Acid levels. Furthermore, the exposure led to an increase in various metabolites in the Tricarboxylic acid cycle of the co-cultivation system, influencing the synthesis and metabolism of key biochemical components like carbohydrates, lipids, and proteins. These findings elucidate the biochemical responses of Chlorella sorokiniana - Aspergillus oryzae co-culture system to pollutants and provide insights into its potential application in the treatment of wastewater containing endocrine disrupting chemicals and heavy metals.
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Analytical Methods
·
2017
·Vol. 9
·期 36
·5356-5364
·
IF 1.9
Y. Wang,S. Q. Jiao,X. L. Chen,T. X. Wei
Herein, an efficient approach towards obtaining molecularly imprinted polymer (MIP) film for the detection of 17β-estradiol (E2) with water-compatible properties using a reversible addition–fragmentation chain transfer (RAFT) via photo-initiation is described. 2-Methyl-2-[(dodecylsulfanylthiocarbonyl)sulfanyl]propanoic acid (DDMAT) as the sole control agent in the absence of additional photoinitiators or catalysts was utilized for the synthesis of MIP film. The MIP film was characterized using contact angle measurements, infrared spectroscopy (IR) and scanning electron microscopy (SEM). Analysis of the surface plasmon resonance (SPR) spectra showed that the imprinted film displayed good sensitivity and selectivity to E2 when compared to other competitors and non-imprinted polymer (NIP) film. The response of the E2 ranged from 10−14 to 10−6 mol L−1 with a limit of detection (LOD) of 1.15 × 10−15 mol L−1 (S/N = 3) in PBS buffer (pH 7.4). This sensor showed good reusability and stability, and retained about 84.8% of its original response after 45 days of storage under dry and ambient conditions. Finally, the sensor was applied to determine the concentration of E2 in tap water and underground water samples in the range from 10−13 mol L−1 to 10−7 mol L−1, and the LODs were obtained as 7.4 × 10−15 mol L−1 and 1.12 × 10−14 mol L−1, respectively.
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NEW JOURNAL OF CHEMISTRY
·
2018
·Vol. 42
·期 4
·2857-2864
·
IF 3.201
Chunxi Zhao,Yang Jiao,Lei Zhang,Yaling Yang
Herein, we report a fast and selective technique for the determination of diethylstilbestrol in milk sample using fluorescent sulfur and boron co-doped carbon dots (S,B co-doped CDs). The S,B co-doped CDs were synthesized by hydrothermal synthesis using poly(sodium-p-styrenesulfonate) and borax as precursors. The as-prepared S,B co-doped CDs possess good stability and fluorescence characteristics and exhibit a fluorescence quantum yield of 25.7%. The fluorescence intensity of the S,B co-doped CDs decreased in the presence of diethylstilbestrol, and a good linear relationship existed between the fluorescence quenching and different concentrations of diethylstilbestrol in the range of 0.1–200 μM with a detection limit of 0.06 μM. Finally, the S,B co-doped CDs were successfully applied in the detection of diethylstilbestrol in milk samples, yielding recoveries between 90.4% and 109.2%.
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JOURNAL OF CHROMATOGRAPHY A
·
2018
·
IF 3.716
Xinyu Liang,Juntao Wang,Qiuhua Wu,Chun Wang,Zhi Wang
A hypercrosslinked triphenylamine polymer (HCTPA) was prepared through a simple one-step Friedel-Crafts alkylation reaction. The HCTPA had an extended π-conjugated system, large specific surface area and high micropore volume. In order to evaluate its extraction performance, the HCTPA was used as the adsorbent for the solid-phase extraction of the phenylurea herbicides (monuron, chlortoluron, isoproturon, monolinuron and buturon) from watermelon, tomato and cucumber samples. The main parameters that could affect the extraction efficiency including the sample volume, sample solution pH, sample solution loading rate and desorption conditions were investigated and optimized. Under the optimized conditions, the HCTPA showed a good extraction performance for the target analytes. The linear range for the quantification of the analytes was in the range of 0.4–160.0 ng g −1 with the correlation coefficients of 0.9996–0.9999. The limits of detection (S/N = 3) of the analytes by the method ranged from 0.06 to 0.12 ng g −1 for watermelon and tomato, and 0.06–0.15 ng g −1 for cucumber samples. The recoveries of the analytes for the method were between 83.1% and 112.5% with the relative standard deviations below 5.5%. These results indicate that the HCTPA can be used for the enrichment of phenylurea herbicides from complex matrix samples like watermelon, tomato and cucumbers.
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