MOLECULES
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2023
·Vol. 28
·期 8
·3542
·
IF 4.6
Qing Liu,Chao Yan,Yan Wang
Applications of submicron-scale particles are of rising interest in separation science due to their favorable surface-to-volume ratio and their fabrication of highly ordered structures. The uniformly dense packing beds in columns assembled from nanoparticles combined with an electroosmotic flow-driven system has great potential in a highly efficient separation system. Here, we packed capillary columns using a gravity method with synthesized nanoscale C18-SiO2particles having diameters of 300–900 nm. The separation of small molecules and proteins was evaluated in the packed columns on a pressurized capillary electrochromatography platform. The run-to-run reproducibility regarding retention time and peak area for the PAHs using a column packed with 300 nm C18-SiO2particles were less than 1.61% and 3.17%, respectively. Our study exhibited a systematic separation analysis of small molecules and proteins based on the columns packed with submicron particles combined with the pressurized capillary electrochromatography (pCEC) platform. This study may provide a promising analytical approach with extraordinary column efficiency, resolution, and speed for the separation of complex samples.Keywords:submicron scale particles;pressurized capillary electrochromatography;separation
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JOURNAL OF MEMBRANE SCIENCE
·
2023
·
IF 9.5
Haojie Zeng,Feiyun Sun,Jianjun Zhang,Ying Wang,Songwen Yang,Dingyu Xing
Polyvinyl alcohol (PVA) has been employed and crosslinked as the selective layer of NF membranes with enhanced hydrophilicity. However, the influences of different crosslinking methods and agents on the reaction mechanism and membrane performance still need to be comprehensively studied. In this study, NF membranes were prepared by coating crosslinking (CC-membrane) and gradient crosslinking (GC-membrane) methods. Compared with CC-membrane, the GC-membrane possessed a 65% higher flux with Na 2 SO 4 rejection around 90%, under the optimal preparation conditions with PVA content of 0.10%, curing at 80 °C for 10 min. Crosslinking agents including 1,3,5-benzenetricarboxylic acid (TMA), 4,4′-(hexafluoroisopropylidene) diphthalic anhydride (6FDA) and pyromellitic dianhydride (PMDA) with different spatial structure were used to optimize the GC-membrane. As confirmed by SEM, XPS, FTIR and contact angle tests, the 6FDA-GC membrane showed a thinner, smoother and more hydrophilic selective layer, and kept an excellent balance between the water flux (88.6 L/m 2 h) and Na 2 SO 4 rejection (88.7%). This is because the 6FDA with a large molecule and flexible spatial structure could form a more integrated crosslinking structure compared to PMDA. Meanwhile, the 6FDA-GC membrane showed rejections of over 80% towards the endocrine-disrupting compound 17α-Ethinylestradiol and exhibited stable antifouling ability and durability. Overall, this work studied systematically the influences of various crosslinking agents on the GC-membrane, and verified the potential of hydrophilic PVA membranes for nanofiltration.
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TALANTA
·
2023
·
IF 6.1
Xuan Ma,Yue Wang,Wenting Wang,Jake Heinlein,Lisa D. Pfefferle,Xuemeng Tian
In this study, a facile method has been developed to synthesize a novel type of porous magnetic molecularly imprinted polymers (Fe 3 O 4 -MER-MMIPs) for the selective adsorption and removal of meropenem. The Fe 3 O 4 -MER-MMIPs, with abundant functional groups and sufficient magnetism for easy separation, are prepared in aqueous solutions. The porous carriers reduce the overall mass of the MMIPs, greatly improving their adsorption capacity per unit mass and optimizing the overall value of the adsorbents. The green preparation conditions, adsorption performance, and physical and chemical properties of Fe 3 O 4 -MER-MMIPs have been carefully studied. The developed submicron materials exhibit a homogeneous morphology, satisfactory superparamagnetism (60 emu g −1 ), large adsorption capacity (11.49 mg g −1 ), quick adsorption kinetics (40 min), and good practical implementation in human serum and environmental water. Finally, the protocol developed in this work delivers a green and feasible method for synthesizing highly efficient adsorbents for the specific adsorption and removal of other antibiotics as well.
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Cell Metabolism
·
2023
·
IF 29
Di Li,Ting Sun,Yongqing Tong,Juan Le,Qian Yao,Jun Tao,Hang Liu,Woer Jiao,Yufeng Mei,Jingru Chen,Zhongchun Liu,Gaohua Wang,Yan Li
Estradiol decline can result in depressive disorders in females; nevertheless, the causes of this decline are unclear. In this study, we isolated estradiol-degrading Klebsiella aerogenes from the feces of premenopausal females with depression. In mice, gavaging with this strain led to estradiol decline and depression-like behaviors. The gene encoding the estradiol-degrading enzyme in K. aerogenes was identified as 3β-hydroxysteroid dehydrogenase (3β-HSD). Heterologously expressing 3β-HSD resulted in Escherichia coli obtaining the ability to degrade estradiol. Gavaging mice with 3β-HSD-expressing E. coli decreased their serum estradiol levels, causing depression-like behaviors. The prevalence of K. aerogene and 3β-HSD was higher in premenopausal women with depression than in those without depression. These results suggest that the estradiol-degrading bacteria and 3β-HSD enzymes are potential intervention targets for depression treatment in premenopausal women.
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Journal of Materials Chemistry B
·
2023
·Vol. 11
·期 22
·4991-4999
·
IF 7
Qingqing Zhou,Yunli Duan,Zhigang Xu,Yu Tian,Zhimin Liu,Chunbo Liu,Pei He,Zhihua Liu,Xiaoxi Si
A kind of selective enrichment material based on a homemade molecularly imprinted polymer (MIP) fiber array with high adsorption capacity was developed for the accurate analysis of estrogens in food samples. Here, the MIP with 17β-estradiol as the template was obtained by in situ polymerization. The chemical composition, morphologies, surface area, and pore size of the polymer were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and Brunauer–Emmett–Teller theory. The extraction time, desorption solvent, desorption time, ionic strength, and the pH of solution were investigated to ascertain the best extraction conditions. Under the optimal extraction conditions, three fiber coatings of 17β-estradiol MIP and commercial polyacrylate (PA) were bound to a homemade handle to assemble the fiber array, respectively. The findings showed that the three-fiber array of the MIP significantly improved the extraction capacity by 145 times compared to PA. The MIP fiber array showed high adsorption capacity for the template molecule 17β-estradiol and its structural analogues estrone, bisphenol F, bisphenol B, and bisphenol A, with enrichment factors of 99.60–133.16. A molecularly imprinted polymer solid-phase microextraction fiber array (MIP-SPME fiber array) coupled with high-performance liquid chromatography-diode array detection was used for the analysis and detection of the five estrogens in milk and yogurt samples. Satisfactory recoveries were achieved ranging from 74.75–119.41% with <9.42% relative standard deviations. The developed method for the simultaneous determination of trace estrogens in food samples exhibited a limit of detection of 0.33 μg L−1. The MIP-SPME fiber array provided an available strategy for improving the selectivity and adsorption capacity of SPME for trace target component analysis in complex matrices and increasing the sensitivity of the analytical method.
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TALANTA
·
2023
·
IF 6.1
Jing Yang,Hao Liu,Yan Huang,Li Li,Xiaoli Zhu,Yaping Ding
Fluorescence carbon quantum dots (CQDs) have been widely applied to sensing and bioimaging. In this paper, near-infrared carbon quantum dots (NIR-CQDs) were prepared through a simple one-step hydrothermal approach using reduced glutathione and formamide as raw materials. Based on NIR-CQDs, aptamer (Apt) and graphene oxide (GO) has been applied to fluorescence sensing cortisol. NIR-CQDs-Apt adsorbed to the surface of GO through π-π stacking and an inner filter effect (IFE) occurred between NIR-CQDs-Apt and GO leading to NIR-CQDs-Apt fluorescence “off”. The IFE process is disrupted in the presence of cortisol, allowing NIR-CQDs-Apt fluorescence “on”. This led us to construct a detection method with excellent selectivity over other cortisol sensors. The sensor can detect cortisol from 0.4 to 500 nM and has a detection limit as low as 0.13 nM. Importantly, this sensor can be used to detect intracellular cortisol with excellent biocompatibility and cellular imaging capabilities, which is promising for biosensing.
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Arabian Journal of Chemistry
·
2023
·
IF 6
Xuhong Cai,Junbo Liu,Dadong Liang,Shanshan Tang,Bao Xu
Combining molecular imprinting technology and quartz crystal microbalance (QCM), the diethylstilbestrol-molecularly imprinted polymers (DES-MIPs) were designed. The LC-ωPBE/6-31G( d , p ) method was chosen to predict the properties of DES-MIPs in this study. The calculated results showed that the complex formed from DES and methacrylic acid with molar ratio of 1:5 and ethylene dimethacrylate as cross-linking agent had the largest amount of hydrogen bonds, the lowest binding energy, and the optimal stability property. With the guidance of calculations, the DES-MIPs were used to prepare QCM electrode by embedding method to construct the DES-MIPs-QCM sensor. The experimental results displayed that the sensor had a high binding affinity for DES when the DES-MIPs was 15 mg and the coating volume was 10 µL. The minimum detection limit of the sensor for DES was 2.63 ng/mL in the range of 50 to 350 ng/mL. The DES-MIPs-QCM sensor exhibited high recognition capacity for DES compared to its structural analogs. The sensor had been successfully used for the determination of DES in the actual water samples.
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MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 12
·1-10
·
IF 6.408
Sun Min,Wang Xiuqin,Ding Yali,Feng Juanjuan
In order to improve the selectivity and stability of melamine–formaldehyde (MF) aerogel, it was composited with TiO 2 aerogel. A TiO 2 -MF hybrid aerogel was in situ prepared on the surface of carbon fibers for in-tube solid-phase microextraction (SPME). The extraction performance of TiO 2 -MF aerogel was regulated by changing the ratio of TiO 2 sol and MF sol during the material preparation. Coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD), the extraction tube filled by TiO 2 -MF aerogel-coated carbon fibers was evaluated with several types of environmental pollutants including polycyclic aromatic hydrocarbons (PAHs), estrogens, and ultraviolet filters. Because of favourable extraction performance of PAHs they were selected as model analytes, and some important influence factors were optimized for satisfactory sensitivity. The detection limits were in the range 0.05–0.10 μg L −1 , owing to high enrichment factors (653–1007). The online in-tube SPME-HPLC–DAD method was verified for the determination of trace PAHs in environmental water samples, and acceptable recovery (70–118%) was achieved. The analytical methods also displayed some advantages in comparison with other reports. Moreover, the extraction tube exhibited satisfactory chemical stability. Graphical abstract
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Separations
·
2022
·Vol. 9
·期 11
·381
·
IF 3.344
Lanbo Bi,Jimin Shen,Zhuoran Yao,Jing Kang,Shengxin Zhao,Pengwei Yan,Binyuan Wang,Zhonglin Chen
In this paper, magnetic molecularly imprinted polymers (MMIPs) were fabricated on the surface of Fe3O4by surface molecular imprinting technology, which can selectively adsorb 17β-estradiol (E2). The optimized experiments demonstrated that MMIPs possessed the best adsorption capacity when methanol was used as the solvent and MAA was used as the crosslinking agent, with a molar ratio of E2: MMA: EGDMA as 1:4:50. SEM, FTIR, and XRD were employed to investigate the morphologies of MMIPs and the results demonstrated that the MMIPs that can selectively adsorb E2 were successfully prepared on Fe3O4particles. The adsorption experiments showed that 92.1% of E2 was adsorbed by the MMIPs, which is higher than the magnetic non-molecularly imprinted polymers (MNIPs). The Freundlich isotherm model was more suitable to describe the adsorption process of E2 by MMIPs. Meanwhile, MMIPs had a better recognition ability for E2 and its structural analogs such as estrone and estriol. The MMIPs still had good adsorption performance after methanol regeneration five times. The prepared MMIPs had the advantages of efficient adsorption ability and high reusability, so they can be applied for selective recognition and removal of E2.Keywords:adsorption kinetics;Fe3O4particles;molecularly imprinted polymers;regeneration process;selective adsorption;17β-estradiol
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Yachao Hao,Wei Zhou,Xin Wang,Youping Liu,Xin Di
In this study, a magnetic graphene oxide modified with green carboxyl-based deep eutectic solvent (MGO@DES) was synthesized for the first time and employed as a highly efficient adsorbent for the magnetic solid-phase extraction (MSPE) of three estrogens in milk samples. With large specific surface, good hydrophobicity and abundant adsorption sites, MGO@DES exhibited excellent extraction performance for estrogens. The adsorption kinetic experiment revealed that 5 mg of MGO@DES reached the equilibrium of estrogen adsorption within 3 min. MGO@DES based MSPE coupled with HPLC-UV method was developed and applied to the determination of three estrogens in milk samples. Good linearity (R 2 > 0.9953) was obtained in the range of 1–200 ng mL −1 and the low limits of detection were 0.20–0.28 ng mL −1 . The spiked recoveries were in the range of 90.3–105.7%, with RSDs less than 7.9%.
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TALANTA
·
2022
·
IF 6.556
Pengfei Zhao,Sisi Tang,Xiaodan Wu,Yu Chen,Kangling Tang,Jinli Fu,Huibin Lei,ZhaoXia Yang,Zhaohui Zhang
Development of method with micro-volume reagent usage and high selectivity for rapid determination of valuable disease-related biomarkers is of great importance for disease surveillance. Herein, a novel ratiometric fluorescence capillary imprinted sensor was developed for highly selective fluorescence determination of sialic acid (SA) based on luminescent metal-organic framework (UiO-66-NH 2 ). In this strategy, the imprinted pre-polymer with double emissions was sucked into the capillary to grow imprinted layer on the inner wall of the capillary. In presence of SA, the blue fluorescence (440 nm) served as fluorescence response signal was quenched due to the electron transfer mechanism between metal organic framework and SA while the red fluorescence (655 nm) served as the reference signal was remained. Within SA concentration linear range of 1.0 × 10 −7 –3.0 × 10 −4 M, the ratiometric fluorescence capillary imprinted sensor was applied to detect SA in human serum and saliva samples successfully with a detection limit of 2.5 × 10 −8 M. A sensitive and selective fluorescence method with micro-volume sample consumption (15 μl) for determination of SA in practical samples was established.
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JOURNAL OF STEROID BIOCHEMISTRY AND MOLECULAR BIOLOGY
·
2022
·
IF 5.011
Liangliang He,Chanjuan Chen,Shuyi Duan,Yang Li,Chuan Li,Xinsheng Yao,Frank J. Gonzalez,Zifei Qin,Zhihong Yao
Xian-Ling-Gu-Bao capsule (XLGB) is a widely prescribed traditional Chinese medicine used for the treatment of osteoporosis. However, it significantly elevates levels of serum estrogens . Here we aimed to assess the dominant contributors of sulfotransferase (SULT) enzymes to the sulfation of estrogens and identify the effective inhibitors of this pathway in XLGB. First, estrone, 17β-estradiol, and estriol underwent sulfation in human liver S9 extracts. Phenotyping reactions and enzyme kinetics assays revealed that SULT1A1 , 1A2, 1A3, 1C4, 1E1, and 2A1 all participated in estrogen sulfation, with SULT1E1 and 1A1 as the most important contributors. The incubation system for these two active enzymes were optimized with Tris-HCl buffer, DL-Dithiothreitol (DTT), MgCl 2 , adenosine 3'-phosphate 5'-phosphosulfate (PAPS), protein concentration, and incubation time . Then, 29 compounds in XLGB were selected to investigate their inhibitory effects and mechanisms against SULT1E1 and 1A1 through kinetic modelling. Moreover, in silico molecular docking was used to validate the obtained results. And finally, the prenylated flavonoids (isobavachin, neobavaisoflavone, etc.) from Psoralea corylifolia L., prenylated flavanols (icariside II) from Epimedium brevicornu Maxim., tanshinones (dihydrotanshinone, tanshinone II-A,) from Salvia miltiorrhiza Bge., and others (corylifol A, corylin) were identified as the most potent inhibitors of estrogen sulfation. Taken together, these findings provide insights into the understanding regioselectivity of estrogen sulfation and identify the effective components of XLGB responsible for the promotion of estrogen levels.
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