ANALYTICAL CHEMISTRY
·
2026
·
IF 7.3
Yifan Li,Junbo Li,Yang Yang,Chunyi Wei,Yuting Song,Bo Jiang,Yunfei Xie,Wei Ji
Exploring the metabolic kinetics mediated by cytochrome P450 (CYP) enzymes is essential for understanding pharmacokinetic and toxicological mechanisms. However, real-time monitoring of CYP-mediated enzymatic reactions remains challenging for conventional techniques. Here, we report the first attempt to develop a surface-enhanced Raman scattering (SERS)-based analytical platform for the direct, real-time tracking of enzymatic metabolism and extraction of critical kinetic parameters. An in vitro CYP enzyme system was constructed to emulate hepatic microsomal activity, using pyrene (Pyr) as a model and polycyclic aromatic hydrocarbon (PAH) as the model substrate. Cetyltrimethylammonium bromide (CTAB)-induced Ag aggregates enabled simultaneous detection of Pyr (408 cm–1) and its metabolite 1-hydroxypyrene (1-OHPyr; 426/617 cm–1) directly within the reaction medium. The hydrophobic CTAB self-assembled monolayer enhanced analyte enrichment and suppressed protein interference, while the intrinsic Raman band of CTAB at 760 cm–1 served as a reliable internal standard for quantitative kinetic assessment. This platform allowed real-time monitoring of CYP-catalyzed oxidation of Pyr, yielding pseudo-first-order kinetics (k = 0.00501 min–1) and the Michaelis constant Km of 13 μM. Furthermore, inhibition studies identified CYP1A2 as the principal isoform responsible for Pyr metabolism, corroborated by the potent inhibitory activity of α-naphthoflavone (with calculated IC50). To our knowledge, this work represents the first instance of SERS for time-resolved monitoring of CYP-mediated metabolism, expanding its capability from static detection to dynamic biochemical analysis. The proposed strategy provides a simple, label-free, and time-resolved approach for enzyme kinetic studies, inhibitor screening, and metabolic analysis.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF APPLIED TOXICOLOGY
·
2023
·
IF 3.3
Miao Yang,Kanmin Mao,Xin Cao,Hongjuan Liu,Xinzheng Wang,Weifeng Mao,Liping Hao
The metabolism of polycyclic aromatic hydrocarbons (PAHs) and the elimination kinetics of their mono-hydroxylated metabolites (OH-PAHs) following single exposure to different combinations of four PAHs (PAH4) were studied. Male Sprague–Dawley rats were orally exposed to a single dose of benzo[a]pyrene (B[a]P) or PAH2 (B[a]P + chrysene), PAH3 (B[a]P + chrysene + benz[a]anthracene), and PAH4 (B[a]P + chrysene + B[a]A + benzo[b]fluoranthene) with each combination adjusted to the same dose of individual compound. OH-PAHs including 3-hydroxybenzo[a]pyrene, 3-hydroxychrysene, 3-hydroxybenz[a]anthracene, and 1-hydroxypyrene (1-OHP) were detected in serum and urine samples collected at six intervals over a 72-h period post-dosing. The hepatic mRNA levels of cytochrome P450 (CYPs) were determined to ascertain the expression induction of PAHs metabolic enzymes. Results showed OH-PAHs (except 1-OHP) peaked within 8 h in serum and were excreted from urine within 24–48 h. The serum and urinary concentration of 3-hydroxybenzo[a]pyrene was significantly increased after PAH4 exposure compared with other PAHs combinations. Inversely, urinary concentration of 3-hydroxychrysene was decreased after PAH4 exposure, and the kinetics of 3-hydroxybenz[a]anthracene or 1-OHP were not different depending on the PAHs combinations. Also, CYPs were markedly induced by PAHs. Notably, the induction levels of CYP1A1 and CYP1B1 were significantly higher after PAH4 exposure compared with B[a]P exposure. The results indicated the metabolism of B[a]P was accelerated after PAH4 exposure which might be partly due to the induction of CYPs. These results confirmed PAHs are rapidly metabolized and suggested potential interactions of PAHs may happen among PAH4 mixture.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF THE ELECTROCHEMICAL SOCIETY
·
2021
·Vol. 168
·期 5
·057509
·
IF 4.316
Yuan Li,Yutong Li,Chao Du,Pengju Zhang,Peipei Cen,Xinsheng Liu,Yonghong Li
Urinary 1-hydroxypyrene (1-OHP) is generally used as an exposure biomarker of polycyclic aromatic hydrocarbons (PAHs). In this work, a colloidal gold modified zeolitic imidazolate frameworks-67/carbon nanofiber paste electrode (Au@ZIF-67/CNFPE) was fabricated for the rapid and sensitive detection of 1-OHP. The morphologies of carbon nanofibers (CNF), ZIF-67, colloidal gold and colloidal gold@ZIF-67 (Au@ZIF-67) were studied by transmission electron microscopy (TEM). The electrochemical behavior of 1-OHP was investigated by square wave voltammetry (SWV). The effect factors like pH value, amount of colloidal gold, accumulation potential and accumulation time have been optimized. Under the optimal conditions, the constructed sensor responded to 1-OHP linearly in the concentration range of 0.0005–10 μM, and the detection limit was 0.1 nM. The reproducibility, stability and selectivity of this sensor were also examined. Finally, the electrode was successfully applied for the analysis of 1-OHP in human urine samples.
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Yuan Li,Yutong Li,Yan Wang,Guodong Ma,Xinsheng Liu,Yonghong Li,Jeffrey Soar
1-hydroxypyrene (1-OHP) is an important biomarker for evaluating human exposure to polycyclic aromatic hydrocarbons (PAHs). In this work, a simple sensor based on nano-carbon paste electrode modified with zeolitic imidazolate frameworks (ZIF-8)/ionic liquid composites was developed for convenient and fast electrochemical detection of 1-OHP. The structure of ZIF-8 and the morphologies of different electrodes were investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The electrochemical behavior of l-OHP on the constructed modified electrode was studied using differential pulse voltammetry (DPV). Under the optimized conditions, the fabricated sensor gave a linear calibration curve of the concentration ranging from 0.05 to 20 μM with a detection limit of 0.01 μM for 1-OHP. The proposed method was successfully applied to the determination of 1-OHP in urine samples with the recoveries of 94.2%–103.2%.
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
·
2020
·
IF 5.065
Jiangping Cao,Qilong Xie,Hongwei Di,Yongfeng Liang,Gui Ma,Zonghui Yi,Ping Zhang,Peng Fu,Jikai Li
A method for the simultaneous determination of eight phenolic compounds (PCs) with a wide polarity range in water samples has been developed and validated using molecular complex based dispersive liquid–liquid microextraction (MC-DLLME) followed by high-performance liquid chromatography. In this process, the molecular complex acted as the extractant, which was formed by tributyl phosphate (TBP) and 1-octanol through hydrogen bond interaction in situ, using a disposable polyethylene pipette for the extraction. The extraction mechanism was investigated by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), which demonstrated that a TBP-1-octanol complex formed via P O HO hydrogen bonding . Furthermore, the extraction mechanism in the dual extraction solvent system involves hydrogen bonding for polar PCs and physical extraction for weak polar and apolar ones. Under the optimum conditions, detection limits were in the range 0.4–5.51 ng/mL and recoveries for the real samples varied from 82.0% to 104.7%, with a relative standard deviation (RSD) of <9.1%. The developed method is simple, inexpensive and sensitive and was successfully applied to the extraction and determination of phenolic compounds in water samples.
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Luping Sun,Shuyun Zhu,Zhenjia Zheng,Jing Sun,Xian-En Zhao,Huwei Liu
Hydroxyl-polycyclic aromatic hydrocarbons (OH-PAHs) are biomarkers for assessing the exposure levels of polycyclic aromatic hydrocarbons (PAHs). A series of stable isotope mass tags (SIMT-332/338/346/349/351/354/360/363/374/377) were firstly designed and synthesized to perform multiplexed stable isotope labeling derivatization (MSILD) of OH-PAHs in human plasma and urine. Their derivatives were enriched and purified by magnetic dispersive solid phase extraction (MDSPE) using prepared Fe 3 O 4 /GO and then determined by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) in multiple reaction monitoring mode. 9-Plexed MSILD reagents were prepared using pipemidic acid as core structure with different isotope mass tags, in which carbonyl chloride group was used to label OH-PAHs. The SIMT-346 labeled OH-PAHs standards were used as internal standards, which can greatly increase the quantitative accuracy. 9-Plex labeled nine different real samples can be quantified by UHPLC-MS/MS in a single run. Under optimized MSILD-MDSPE conditions, good linearities of seven OH-PAHs were obtained with satisfactory coefficient of determination R 2 > 0.991. Limits of detection (LODs) of seven OH-PAHs were from 0.1 to 0.5 pg/mL, and limits of quantitation (LOQs) ranged from 0.5 to 2.0 pg/mL. The intra- and inter-day precisions ranged in 2.3–12.4% with accuracies in the range of 91.7–108.4%. Acceptable results of matrix effect (89.7–105.7%) and derivatization efficiency (> 96.4%) were obtained. In short, the developed method has been proved to be high-throughput, sensitive, accurate and easy-handling. This method was applied for the measurement of seven free OH-PAHs in human urine and plasma, and expected to provide technical support for the evaluation of PAHs exposure levels in humans.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 11
·1-9
·
IF 5.479
Xue Jin-Hua,Liu Ling,Wang Yong-Sheng,Li Jia-Qian,Li Mei,Qu Yue-Ning,Li Le
This work describes a method for the determination of 1-hydroxypyrene (OH-Py) via aggregation-induced quenching of the emission of protamine-coated gold nanoclusters using 9-hydroxyphenanthrene (OH-Phe) as a sensitizer to boost the emission efficiency of nanoprobe. Under optimum conditions, the drop in fluorescence intensity at excitation/emission wavelengths of 300/596 nm is proportional to the concentrations of OH-Py in the range from 1.0 to 65 nM. The relative standard deviations are 4.2, 2.4 and 1.9% (for n = 11) at concentration levels of 8.0, 32 and 48 nM of OH-Py, respectively. The detection limit is 0.3 nM which is much lower than that of some previously reported methods. The recoveries from urine samples spiked with OH-Py ranged between 94.4 and 98.8%.
1-Hydroxypyrene (OH-Py) can trigger the aggregation of protamine-gold nanoclusters (PRT-AuNCs), resulting in the emission quenching of PRT-AuNCs. 9-Hydroxyphenanthrene (OH-Phe) can boost the emission efficiency of nanoprobe. Thereby, a highly sensitive assay of OH-Py was established.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
SENSORS AND ACTUATORS B-CHEMICAL
·
2019
·
IF 6.393
Long Yu,Qutong Zheng,Di Wu,Yuxiu Xiao
pH is of great importance in understanding physiological and pathologic processes. Abnormal gastric juice pH is an indicator of many gastric diseases such as peptic ulcer and gastric cancer. In this work, a nanocomposite 1-hydroxypyrene@ Co/Tb- dipicolinic acid metal-organic framework (1-OHP@Co/Tb-DPA MOF) was constructed as a ratiometric fluorescent pH sensor for strong acidity. The nanocomposite-based pH sensor was response-rapid (30 s), linearly responsive in the broad pH range of 0.3–7.8 ( r > 0.95) and ultra-sensitive in the pH range of 0.3–5.0. Importantly, the nanocomposite-loaded fiber paper was prepared as a visual microsensor for point-of-care pH detection via ratiometric chromaticity, coupled with a homemade portable determination device. The paper-based visual microsensor is response-rapid and sensitive, long-term stable (at least 30 days), and suitable for pH assay of microvolume (as little as 5 μL) samples at pH 0.3–5.0. Both the nanocomposite-based ratiometric fluorescent sensor and the paper-based visual microsensor can accurately determine the pH of artificial gastric juices (relative error <5.4%). To our knowledge, this is the first time to report a MOF-based ratiometric fluorescent pH sensor for strong acidity (pH<1) and a paper-based pH microsensor for point-of-care visual assay via ratiometric chromaticity.
✓ 已验证
产品关联
DOI
高影响因子
CHEMICAL RESEARCH IN CHINESE UNIVERSITIES
·
2015
·Vol. 31
·期 2
·224-227
·
IF 0.875
Zhang Ran,Xu Lihua,Chen Hui,Qin Zhihong,Zhao Yu,Ni Zhonghai
1-Thiohydroxypyrene( 1 ) and its two intermediates, 1-pyrenyl- O -thiocarbamate( 2 ) and 1-pyrenyl- S -thiocarbamate( 3 ), were synthesized using 1-hydroxypyrene as the starting material. The key synthetic step is Newman-Kwart rearrangement. The results indicate that the Newman-Kwart rearrangement is more effective in suitable solvent than conventional method based on pure organic compound. The structures of compounds 1 – 3 were characterized by FTIR, NMR, GC-MS and elementary analysis. The crystal structures of two new compounds( 2 and 3 ) were determined by single crystal X-ray diffraction analysis. The whole synthetic process is simple, mild and with high yield.
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2016
·
IF 5.886
Langjun Zhou,Yuling Hu,Gongke Li
Conjugated microporous polymers (CMPs), linked by a covalent bond to form an extension of the aromatic ring skeleton, are microporous materials characterized by a highly conjugated structure and high stability. The present study reported on a novel strategy for the synthesis of CMPs with built-in magnetic nanoparticles for excellent enrichment of trace hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) in human urine. We modified Fe3O4 nanoparticles with boronic acid groups and then reacted the nanoparticles with reactive monomers of polyphenylene conjugated microporous polymer (PP-CMP) to anchor the magnetic components in the PP-CMP framework. Chemical bonding between Fe3O4 nanoparticles and PP-CMP networks, together with equally firm covalent linkage and rigidity of the PP-CMP network, endows the magnetic PP-CMP with remarkable chemical stability and durability, even in harsh conditions. Magnetic PP-CMP has the characteristics of high conjugation ability, highly porous structure, and magnetism, which makes it an ideal magnetic adsorbent for trace analytes with aromatic conjugation structure. The adsorption mechanism of OH-PAHs on magnetic PP-CMP was investigated and demonstrated that hydrophobic interaction was important for the contribution of interaction between adsorbents and target analytes, together with the assistance of π–π stacking interaction. For the application, the magnetic PP-CMP was used for the enrichment of trace OH-PAHs in human urine of both smokers and nonsmokers in combination with high-performance liquid chromatography with fluorescence detection (HPLC-FLD). It showed good selectivity and excellent sensitivity to these OH-PAHs. Their detection limits were low and in the range of 0.01–0.08 μg·L–1. The OH-PAHs were detected with different amounts from 0.054 to 0.802 μg·L–1 in urine samples from smokers and nonsmokers. The recoveries were found to be 76.0%–107.8%. The results indicate that the magnetic PP-CMP offers an efficient enrichment method for trace OH-PAHs in human urine.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Haidong Gao,Shucai Gao,Ming Lv,Yeru Liu,Jingjing Yao,Hongwei Liu,Fayun Wang,Mantang Chen,Libin Wan
Polycyclic aromatic hydrocarbons (PAHs) have been classified as the earliest discovered class of environmental carcinogens, seriously endangering human health and ecological safety, and the hydroxylpolycyclic aromatic hydrocarbons (OH-PAHs) in human urine are considered as the main biomarkers to evaluate the exposure levels of PAHs in human body. Therefore, it is necessary to develop an accurate and sensitive method for the determination of urinary OH-PAHs. Herein, we proposed electromembrane extraction (EME) as a simple, effective and ecofriendly sample pretreatment technique for selective extraction, purification and enrichment of four typical OH-PAHs (2-naphthol, 2- and 3-phenanthrol, 2-hydroxyfluorene) in human urine for the first time. Under the optimum conditions, an analytical method of EME coupled with HPLC was established, which provided wide linear ranges for four OH-PAHs from 1 to 500 ng mL -1 with low LODs of 0.05–0.3 ng mL -1 . The average recoveries of four OH-PAHs at three spiked levels in human urine were 81.6–102.5% with RSDs all below 9.4%. The present method has been successfully applied for the sensitive determination of trace four OH-PAHs in urine samples from non-smokers and smokers with a maximum concentration of 2.24 and 3.56 ng mL -1 , respectively, which showed a great potential for the analysis of trace OH-PAHs in biological samples.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2025
·
IF 9
Zhuo Chen,Zhiyang Lu,Weijun Tian,Bingkun Liu,Bingjie Huo,Jing Zhao,Mengyuan Zou,Ruijuan Zhang,Xinran Yu,Xinbo Wang
Pyrene (Pyr) and its derivatives are classified as Persistent Organic Pollutants (POPs), which exhibit significant toxicological effects and pose serious threats to ecosystems. Photocatalytic technology is increasingly employed for the remediation of POPs due to its effective and environmentally sustainable degradation capabilities. However, conventional photocatalytic materials, primarily in powder form, face challenges related to separation and recovery from aqueous environments, significantly limiting their practical application. In this study, we successfully synthesized a three-dimensional (3D) porous immobilized photocatalytic material by decorating Ag 3 PO 4 and BiOBr onto Ni foam (NF) using a hydrothermal method combined with continuous ionic layer adsorption. The results demonstrated Ag 3 PO 4 /BiOBr/NF exceptional light degradation capabilities, achieving over 90 % degradation of Pyr, 1-methylpyrene, and 1-hydroxypyrene, as well as over 40 % degradation of 1-nitropyrene under visible light irradiation over a duration of 5 h. Its degradation efficiency decreased by 12.49 % after five cycles, demonstrating its reusability. The roles of superoxide radicals ( O 2 – ) and holes (h + ) were critical in the degradation process. Furthermore, based on experimental findings, we proposed a Z-type heterojunction degradation mechanism for the Ag 3 PO 4 /BiOBr/NF composite, accompanied by an analysis of the potential degradation pathways for Pyr. Consequently, the recyclable immobilized photocatalytic materials developed in this research contribute novel insights into the photocatalytic degradation of POPs.
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）