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ANALYTICA CHIMICA ACTA · 2024 · IF 5.7

Ultrasensitive mass spectrometric quantitation of apurinic/apyrimidinic sites in genomic DNA of mammalian cell lines exposed to genotoxic reagents

Chen-Yu Xue,Ya-Hong Liu,Yue Yu,Ying Liu,Ying-Lin Zhou,Xin-Xiang Zhang

The apurinic/apyrimidinic (AP) site is an important intermediate in the DNA base excision repair (BER) pathway, having the potential of being a biomarker for DNA damage. AP sites could lead to the stalling of polymerases, the misincorporation of bases and DNA strand breaks, which might affect physiological function of cells. However, the abundance of AP sites in genomic DNA is very low (less than 2 AP sites/10 6  nts), which requires a sensitive and accurate method to meet its detection requirements. Here, we described an ultrasensitive quantification method based on a hydrazine- s -triazine reagent (i-Pr 2 N) labeling for AP sites combining with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The limit of detection reached an ultralow level (40 amol), realizing the most sensitive MS-based quantification for the AP site. To guarantee the accuracy of the quantitative results, the labeling reaction was carried out directly on DNA strands instead of labeling after DNA enzymatic digestion to reduce artifacts that might be produced during the enzymatic process of DNA strands. And selective detection was realized by MS to avoid introducing the false-positive signals from other aldehyde species, which could also react with i-Pr 2 N. Genomic DNA samples from different mammalian cell lines were successfully analyzed using this method. There were 0.4–0.8 AP sites per 10 6 nucleotides, and the values would increase 16.1 and 2.75 times when cells were treated with genotoxic substances methyl methanesulfonate and 5-fluorouracil, respectively. This method has good potential in the analysis of a small number of cell samples and clinical samples, is expected to be useful for evaluating the damage level of DNA bases, the genotoxicity of compounds and the drug resistance of cancer cells, and provides a new tool for cell function research and clinical precise treatment.

CAS / MDL: 1336-21-6
研究领域: 分子生物学 · 分析化学 · 毒理学 · 药理学 · 临床研究
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JOURNAL OF CELLULAR AND MOLECULAR MEDICINE · 2020 ·Vol. 24 ·期 9 ·5168-5184 · IF 4.486

A network pharmacology-based approach to explore the effects of Chaihu Shugan powder on a non-alcoholic fatty liver rat model through nuclear receptors

Huan Nie,Yuanjun Deng,Chuiyang Zheng,Maoxing Pan,Jiqian Xie,Yupei Zhang,Qinhe Yang

The pathogenesis of non-alcoholic fatty liver disease (NAFLD) is still not fully understood, and currently, no effective pharmacotherapy is available. Nuclear receptors (NRs) are important biological participants in NAFLD that exhibit great therapeutic potential. Chaihu Shugan powder (CSP) is a traditional Chinese medicine (TCM) formula that has a wide therapeutic spectrum including NAFLD, but the effective components and functional mechanisms of CSP are unclear. We adopted a network pharmacology approach using multiple databases for Gene Ontology (GO) enrichment analysis and the molecular complex detection (MCODE) method for a protein-protein interaction (PPI) analysis, and we used molecular docking method to screen the NR targets and determine the corresponding CSP components. The screening results were validated through a NAFLD rat model that was used to explain the possible relationship between CSP and NAFLD. Finally, we screened PPARγ, FXR, PPARα, RARα and PPARδ as target genes and quercetin , kaempferol , naringenin , isorhamnetin and nobiletin as target compounds. The five components were detected through high-performance liquid chromatography-mass spectrometry (HPLC-MS), the results of which aligned with the docking experiments of PPARγ, PPARα and PPARδ. After CSP intervention, the NAFLD rat model showed ameliorated effects in terms of bodyweight, hepatic histopathology, and serum and liver lipids, and the mRNA levels of PPARγ, FXR, PPARα and RARα were significantly changed. The results from this study indicate that CSP exhibits healing effects in an NAFLD model and that the network pharmacology approach to screening NR targets and determining the corresponding CSP components is a practical strategy for explaining the mechanism by which CSP ameliorates NAFLD.

研究领域: 药理学 · 中药学 · 分子生物学 · 病理学
✓ 已验证 DOI PubMed 高影响因子
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 5 ·1-9 · IF 5.479

Simultaneous HPLC-MS determination of 8-hydroxy-2′-deoxyguanosine, 3-hydroxyphenanthrene and 1-hydroxypyrene after online in-tube solid phase microextraction using a graphene oxide/poly(3,4-ethylenedioxythiophene)/polypyrrole composite

Chen Dan,Xu Hui

The exploration of monohydroxy polycyclic aromatic hydrocarbons and 8-hydroxy-2′-deoxyguanosine (8-OHdG) produced by oxidative stress and DNA damage is a powerful and non-invasive tool to study the health risk of exposure to polycyclic aromatic hydrocarbons (PAHs). A nanocomposite prepared from graphene oxide, poly(3,4-ethylenedioxythiophene) and polypyrrole was electrodeposited on the internal surface of a stainless-steel tube for online in-tube solid phase microextraction (IT-SPME) of 8-OHdG, 3-hydroxyphenanthrene and 1-hydroxypyrene from urine. The coating possesses excellent chemical and mechanical stability, high extraction efficiency, good resistance to matrix interference, and a long lifespan. An online IT-SPME-high performance liquid chromatography-mass spectrometry method was developed for the determination of these three metabolite biomarkers in human urine. Figures of merit include (a) enrichment factors of 30–48; (b) low limits of detection (4–41 pg·mL −1 at S/ N  = 3); (c) wide linear ranges (0.05–50 ng·mL −1 ); (d) good recoveries from spiked samples (71.6–109.5%); and (e) acceptable repeatability (2.3–14.6%). The method offers the advantages of low cost, simplicity, sensitivity, rapidity and automation. Schematic illustration of online in-tube solid phase microextraction using graphene oxide/poly(3,4-ethylenedioxythiophene)/polypyrrole composites as adsorbent in a stainless-steel (SS) tube for the enrichment and simultaneous determination of 8-hydroxy-2′-deoxyguanosine, 3-hydroxyphenanthrene and 1-hydroxypyrene prior to HPLC-MS analysis.

研究领域: 分析化学 · 环境健康 · 毒理学
✓ 已验证 DOI PubMed 高影响因子
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment · 2020 · IF 2.34

Development and establishment of a QuEChERS-based extraction method for determining tembotrione and its metabolite AE 1417268 in corn, corn oil and certain animal-origin foods by HPLC-MS/MS

Kai Cui,Xiaohu Wu,Lusheng Zhu,Ying Zhang,Gaochen Dai,Junli Cao,Jun Xu,Fengshou Dong,Xingang Liu,Yongquan Zheng

In this study, we established a rapid and sensitive HPLC-MS/MS method for quantitative determination of tembotrione and its metabolite AE 1417268 (M5) in corn, corn oil, beef, pork, chicken, and eggs. Both analytes eluted from a C18 column within 6 min. The electrospray ionisation–positive mode was used for tembotrione, whereas the negative mode was used for M5. Acetonitrile was the extractant for all samples, and the addition of 2 g NaCl to each homogenised sample facilitated the extraction of the analytes into acetonitrile. The extracted analytes were further purified by the addition of 50 mg of C18 sorbent (25 mg GCB was also added to corn samples) for subsequent HPLC-MS/MS analysis. Satisfactory calibration-curve linearities (R2 ≥ 0.997) were obtained for the two analytes at concentrations of 1–500 μg/L. Mean recoveries in different matrices ranged from 73.7% to 110.4%, whereas intra-day and inter-day relative standard deviations were <15% for all concentrations of spiked analytes. The limit of quantification was 2 μg/kg for each analyte in all matrices. In food samples obtained from markets, residual tembotrione and M5 were all below the limits of quantification. These results confirm that the method is suitable for the routine monitoring of residual tembotrione and M5 in a variety of food matrices.

研究领域: 食品科学 · 分析化学
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ANALYTICAL LETTERS · 2022 · IF 2.267

Determination of Paralytic Shellfish Toxins in Bivalve Mollusks by Amino-Modified Multiwalled Carbon Nanotube (MWCNT) Solid-Phase Extraction (SPE) and High-Performance Liquid Chromatography–Tandem Mass Spectrometry (HPLC–MS/MS)

Xu-Feng Wang,Qiang Wang,Jin-Lan Yang,Dong-Hao Zhao

An amino-modified multiwalled carbon nanotube (MWCNT) solid-phase extraction-based hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC–MS/MS) method was developed for simultaneous determination of 13 paralytic shellfish toxins (PSTs) in bivalve mollusks. Shellfish samples were extracted with 1% acetic acid followed by cleanup using optimized MWCNT-NH2 based solid-phase extraction. Absorbed PSTs were eluted with 2 mL 1% acetic acid–acetonitrile (70/30, v/v). The separation was performed on a Waters BEH Amide column within 7.5 min utilizing 0.1% formic acid–acetonitrile and 2 mM ammonium acetate containing 0.1% formic acid as the mobile phase. The analytes were quantified by matrix-matched external standard curves with correlation coefficients® exceeding 0.997 acquired in multiple reaction-monitoring mode. The limits of detection and quantitation in shellfish samples were from 2.76 to 9.8 μg/kg and 9.11 to 39.3 μg/kg, respectively. Recoveries at three spiked levels ranged from 71.4% to 97.8% with relative standard deviations less than 12.6%. The developed method was satisfactorily applied to the analysis of shellfish.

CAS / MDL: 308068-56-6
研究领域: 分析化学 · 食品安全
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2023 · IF 3

Development and validation of an HPLC-MS/MS method for the simultaneous analysis of volatile organic compound metabolites, hydroxylated polycyclic aromatic hydrocarbons, and 8-hydroxy-2′-deoxyguanosine in human urine

Rong-Fa Xu,Hang Mei,Li Chen,Bin Tang,Qi-Yuan Lu,Feng-Shan Cai,Xiao Yan,Jing Zheng,Xian-Tao Shen,Yun-Jiang Yu

Humans are widely and concurrently exposed to volatile organic compounds (VOCs) and polycyclic aromatic hydrocarbons (PAHs). However, few studies have reported the internal co-exposure levels of these chemicals in occupational and general populations. Specifically, the associations revealed between the urinary levels of metabolites of VOCs (mVOCs), hydroxylated PAHs (OH-PAHs), and oxidative stress biomarkers for humans remain limited. In this study, a method based on solid-phase extraction (SPE) and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous analysis of 22 mVOCs, 12 OH-PAHs, and 8-hydroxy-2′-deoxyguanosine (8-OHdG) in human urine samples. The method was validated with all target analyte accuracies and precisions in the range of 76 %–120 % and 1 %–14 % at three levels of spiked urine samples, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the target analytes were 0.01–0.34 ng/mL and 0.01–7.57 ng/mL, respectively. And the method was applied to measure urinary levels of target analytes from 38 petrochemical workers in Guangzhou, South China. Except for 3-hydroxy-benzo[a]pyrene, all target analytes were detected in the urine samples. The average levels were 0.05–12.6 ng/mL for individual OH-PAHs, 0.20–73620 ng/mL for individual mVOCs, and 1.00 ng/mL for 8-OHdG. Additionally, 3-hydroxy-phenanthrene, 1-hydroxy-pyrene, 6-hydroxy-chrysene, N-acetyl-S-(trichlorovinyl)-L-cysteine, 2-methylhippuric acid, thiodiacetic acid, trans, trans -Muconic acid, and N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine had statistically significant positive effects on 8-OHdG levels, while 1-hydroxy-naphthalene, 1,2-dihydroxybenzene, and hippuric acid showed a negative effect on 8-OHdG, indicating these metabolites could lead to synergistic or antagonistic oxidative DNA damage. This study provides a robust analytical method that permits a comprehensive assessment of co-exposure to PAHs and VOCs and their potential adverse health effects.

CAS / MDL: 88847-89-6
研究领域: 环境科学 · 毒理学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Bioscience · 2025 · IF 5.9

Changes of Unique Flavor Substances and Metabolic Pathway Brought by Lacticaseibacillus rhamnosus WH. FH-19 Fermented Milk during Fermentation and Storage Stage: HS-SPME-GC-MS and HPLC-MS-based Analysis

Lu Feng,Jingxia Yang,Liping Sun,Xiaoyan Zhu,Wei Lan,Guangqing Mu,Xuemei Zhu

We evaluated the changes in volatile and nonvolatile flavor substances after fermented milk was fermented by Lacticaseibacillus rhamnosus WH. FH-19 using Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) and High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). The results have shown that the addition of L. rhamnosus WH. FH-19 can increase the contents of acetoin and 2-nonanone which can give fermented milk cream and cheese flavor, and significantly enrich amino acid metabolism and carbon metabolism. The fermentation of L. rhamnosus WH. FH-19 increased the contents of L-glutamic acid, taurine, stachyose, erythritol, L-rhamnose, retinol, pantothenic acid and 19 oligopeptides in fermented milk, and endowed fermented milk with good flavor, quality and antioxidant capacity. The results presented that L. rhamnosus WH. FH-19 can increase the content of flavor substances, promote the metabolism of amino acids and carbohydrates in fermented milk, and produce more antioxidant metabolites, which had the potential as a starter of fermented milk.

CAS / MDL: 367-11-3
研究领域: 食品科学 · 微生物学
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CHEMICAL ENGINEERING JOURNAL · 2023 · IF 15.1

G-C3N4 with gradient vacancies to enhance spatial charge carriers transfer and separation for photodegrading antibiotics under visible light

Xingyu Zhan,Yunxiong Zeng,Zhilong Zhang,Yingchun Xia,Jingcai Xu,Bo Hong,Xinqing Wang

Antibiotic pollution has potential toxicities to living organisms and the ecological environment and draws great concern of researchers. Photocatalytic degradation of antibiotics by g-C 3 N 4 shows an unsatisfied activity due to the low utilization efficiency of photogenerated electrons and severe charge recombination. A main reason is the neglect of the utilization of electrons at the depth of the material surface. Herein, we report local microenvironment rearranged g-C 3 N 4 (V C, N -CN 6 ) with intrinsic gradient concentration nitrogen (V N ) and carbon vacancy (V C ) via KBH 4 etching followed by water oxidation, enabling a complete photocatalytic degradation (≥99.6%) of TC within 3 min under visible light. This photoactivity has a universality, and can completely visible-light photodegrade sulfadiazine and ciprofloxacin in a short time. Such an extraordinary activity is ascribed to cooperation between gradient V N modulating utilization of internal electron and V C enhancing reactive species generation. Additionally, photodegraded pathways, intermediates, and risks of TC photocatalytic degradation were elucidated by the HPLC-MS and quantitative structure-effect relationship mathematical model. This work enriches the toolbox to engineer the local microenvironment of photocatalysts to upgrade the utilization of internal photoexcited electrons and heighten TC photocatalytic degradation efficiency.

研究领域: 环境科学 · 材料科学 · 化学 · 光化学 · 催化
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MOLECULES · 2018 ·Vol. 24 ·期 1 ·64 · IF 3.098

Simultaneous Determination of Five Phenolic Acids and Four Flavonoid Glycosides in Rat Plasma Using HPLC-MS/MS and Its Application to a Pharmacokinetic Study after a Single Intravenous Administration of Kudiezi Injection

Peiying Shi,Chunlei Yang,Ya Su,Liying Huang,Xinhua Lin,Hong Yao

This study has developed a reliable and precise high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of five phenolic acids and four flavonoid glycosides in rat plasma after a single intravenous administration of Kudiezi injection (KI). Chromatographic separation was carried out on an Ultimate®XB-C18column (4.6 × 100 mm, 3.5 μm) using a gradient elution program with a mobile phase consisting of water containing 0.5% acetic acid and acetonitrile at a flow rate of 0.6 mL/min. Detection was performed on a triple-quadrupole tandem mass spectrometry using multiple reaction monitoring in negative electrospray ionization mode. The calibration curves of all analytes showed good linearity (R2> 0.990). The results of selectivity, intra-day and inter-day precisions, extraction recoveries, matrix effects and stability were satisfactory. Pharmacokinetic parameters showed that luteolin-7-O-β-d-gentiobioside, luteolin-7-O-β-d-glucuronide, luteolin-7-O-β-d-glucoside and apigenin-7-O-β-d-glucuronide were eliminated quickly (0.07 h

CAS / MDL: 64-19-7
研究领域: 药理学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Polymers · 2022 ·Vol. 14 ·期 21 ·4682 · IF 4.967

Development and Evaluation of a Novel Sulfonated Phenol–Formaldehyde Resin with High Dispersion Stability

Xianxing Meng,Likun Wang,Hongwei Wang,Fang Zhang,Taying Su,Kunmu Cheng

Sulfonated phenol–formaldehyde (SPF) resin used as a cross-linker for petroleum reservoir conformance control was synthesized under alkaline conditions. The reaction process of SPF resin was evaluated by measuring the solution’s viscosity with respect to phenol–formaldehyde (PF) resin. The molecular structure of SPF resin was characterized by both FTIR and HPLC–MS/MS. The influence of the formaldehyde/phenol molar ratio (F/P) and the sodium formaldehyde sulfoxylate/phenol molar ratio (S/P) on the properties of SPF were analyzed in terms of the storage time, coagulation value, molecular size, and zeta potential. The results indicate that the presence of formaldehyde sodium bisulfite could slow down condensation reaction. Phenol rings were connected by methylene bridges in the position of o–p, and sulfonated SPF resin molecules all had one sulfonate group on the oligomer structure. The storage time decreased from 87 to 6 days, and the zeta potential decreased from −3.02 to −7.70 mV with the increase in F/P (1.2–2.0). Meanwhile, the sedimentation value and the diameter increased from 3.291 × 104to 5.045 × 104mg/L and from 2.7 to 5.3 nm, respectively. Sulfonation could significantly increase the storage time and dispersion stability. With the increase in S/P (0.1–0.35), the storage time increased from 15 to 86 days, the sedimentation value increased from 1.927 × 104to 5.269 × 104mg/L, and the diameter decreased from 6.3 to 3.0 nm. This paper can present new ideas for improving the storage stability and salt tolerance of phenol–formaldehyde resin and further improving the range of its applications, which has essential reference significance.Keywords:phenol–formaldehyde resin;sulfonation;characterization;HPLC–MS/MS

CAS / MDL: 108-95-2 50-00-0
研究领域: 化学工程 · 石油工程 · 材料科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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International Journal of Electrochemical Science · 2023 · IF 1.5

Enhanced degradation of quinoline in three-dimensional electro-Fenton system using catalytic Fe-Co-Ni-P/g-C3N4 particles

Jun Chen,Boding Zhang,Bingxing Wang,Chengxing Cui,Songlin Wang,Jichao Wang,Wenlong Zhang

With high toxicity, carcinogenicity and teratogenicity, quinoline has been threatening human health and ecological environment. Herein, Fe-Co-Ni-P/g-C 3 N 4 particles are developed as electrochemical reactors to form a three-dimensional catalytic particle electrode system (3D-CPE) for efficient removal of quinoline from wastewater by electro-Fenton (EF) oxidation process. with reaction time of 30 min, the particles dosage of 50 g/L, pH of 3, conductivity of 11.5 ms/cm, and current density of 37.04 mA/cm 2 , the chemical oxygen demand (COD) removal rate can up to 90.95%. In addition, electron paramagnetic response (EPR) and radical scavenging tests are performed to determine the hydroxyl radicals of electrochemical processes produced. The degradation products are analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS). Finally, through theoretical calculation and analysis of degradation products, a reasonable degradation mechanism is proposed.

研究领域: 环境科学 · 化学工程 · 水处理 · 电化学
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JOURNAL OF HAZARDOUS MATERIALS · 2025 · IF 11.3

Sustainable One-Pot Synthesis of Dual-Mechanism Magnetic HCPs for Classified Extraction of Trace PAHs and Quaternary Ammonium Pesticides in Environmental Waters

Xue Ma,Mengmeng Fu,Kai Hu,Li Gao,Chenchen Song,Shusheng Zhang,Renyong Zhao,Wenjie Zhao

Developing efficient and reliable adsorbents with simplified synthesis and mixed-mode performance is crucial for the accurate quantitative analysis of diverse coexisting environmental pollutants. A magnetic carboxylated hypercrosslinked organic polymer (Fe 3 O 4 /HCP-COOH) with reverse phase/cation exchange mixed-mode performance was synthesized through a two-stage process: (1) Fabrication of HCP-COOH via FeCl 3 -catalyzed Friedel-Crafts alkylation using 1,4-phenylenediacetic acid and 1,4-bis(chloromethyl)benzene; (2) In situ growth of Fe 3 O 4 nanoparticles on HCP-COOH through coprecipitation, utilizing FeCl₃ dually as polymerization catalyst and iron precursor to enhance process efficiency and waste minimization. The nanocomposite functioned as a mixed-mode sorbent for magnetic solid-phase extraction (MSPE), integrating dual retention mechanisms to selectively extract hydrophobic polycyclic aromatic hydrocarbons (PAHs) and cationic quaternary ammonium pesticides (QUATs), with subsequent analysis by GC-MS for PAHs and HPLC-MS/MS for QUATs respectively. Following optimization of adsorption pH, eluent composition, and contact time, the method exhibited high sensitivity with limits of detection (LODs) of 0.80-7.93   ng   L⁻¹ for 15 PAHs and 0.02-16.31   ng   L⁻¹ for 4 QUATs. Validation showed satisfactory recoveries of 89.5-98.3% (RSDs ≤11.2%) in snowmelt and 90.4-101.8% (RSDs ≤11.6%) in lake water (n=3), confirming practicality for simultaneous monitoring of hydrophobic and cationic contaminants in complex environmental water, offering significant advantages in multi-residue analysis for environmental monitoring applications.

研究领域: 环境化学 · 分析化学 · 材料科学 · 污染监测 · 可持续合成
✓ 已验证 产品关联 DOI PubMed 高影响因子
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