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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2018 · IF 2.88

Determination of diclofenac sodium by resonance light scattering method using silver nanoparticles as probe

Tao Liu,Zhihai Xie,Qing Liu

A sensitive, simple and novel method was developed to determine diclofenac sodium (DS) using silver nanoparticles (AgNPs) as probe by resonance light scattering (RLS) technique. It was found that DS could quench the RLS intensity of AgNPs . Moreover, the decrease in RLS intensity was linearly correlated to the concentration of DS over the range of 0.01–2.0   μg   mL −1 . DS can be measured in a short time (5   min) without any complicated or time-consuming sample pretreatment process. Parameters that affect the RLS intensities such as pH, concentration of AgNPs, reaction time, electrolyte concentration , and coexisting substances were systematically investigated and optimized. The results showed that the method had a very good selectivity and could be used conveniently for the determination of DS. The limit of detection (LOD) was 2.85   ng   mL −1 (3σ), and the relative standard deviation (RSD) was less than 3.6% ( n   =   6). Possible mechanism for the RLS changes of AgNPs in the presence of DS was discussed and the method was successfully applied for the analysis of tablets and urine samples.

研究领域: 分析化学 · 纳米技术 · 药物分析 · 环境监测
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JOURNAL OF MOLECULAR STRUCTURE · 2026 · IF 4.9

Structural and physicochemical evaluation of three amine salts of diclofenac with improved aqueous solubility

Xian-Rui Zhang,Xian-Ying Xie,Yan Liu,Lu-Ting Jiang,Hong-Mei Yang,Lei Gao

This study aimed to overcome the poor aqueous solubility of diclofenac (DIC), a BCS Class II drug, through the strategic formation of amine salts. Three novel salts with diisopropylamine (DIP), butanolamine (BUTA), and tromethamine (TRIS) were successfully synthesized and comprehensively characterized. Single-crystal X-ray diffraction revealed distinct hydrogen-bonded networks for each salt, ranging from cyclic tetramers (DIC-DIP) to extended three-dimensional frameworks (DIC-BUTA, DIC-TRIS). Solid-state characterization by PXRD, DSC and FTIR spectroscopy confirmed the formation of new, phase-pure crystalline materials, with FTIR clearly showing the disappearance of the carboxylic C=O band and the appearance of carboxylate bands, confirming proton transfer. The salts demonstrated dramatically enhanced equilibrium solubility and intrinsic dissolution rates (IDR) compared to the parent DIC, particularly in water. The most significant improvements were observed for DIC-BUTA and DIC-DIP, achieving solubility increases of 213.0-fold and 146.4-fold, and IDR increases of 276.0-fold and 222.7-fold, respectively. The superior dissolution performance of DIC-BUTA and DIC-DIP is correlated with their moderate hydrogen-bond networks (5 and 3 donor bonds, respectively) and lower crystal densities (1.326 and 1.262 g/cm³), which facilitate easier lattice disruption and solvation. Conversely, the densely packed, highly hydrogen-bonded structure of DIC-TRIS resulted in the highest lattice stability but the most modest solubility enhancement. All salts exhibited congruent dissolution without phase transformation. This work establishes DIC-BUTA and DIC-DIP as the most promising candidates for developing rapid-release oral formulations of diclofenac and provides fundamental insights into the structure-property relationships governing salt solubility.

CAS / MDL: 15307-86-5
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CHEMICAL ENGINEERING JOURNAL · 2021 · IF 13.273

Ru doped graphitic carbon nitride mediated peroxymonosulfate activation for diclofenac degradation via singlet oxygen

Ying Yan,Qinxue Yang,Qigao Shang,Jing Ai,Xiaofang Yang,Dongsheng Wang,Guiying Liao

Metals doped carbon nitride (CN) is considered as a class of promising efficient catalysts for peroxymonosulfate (PMS) activation in water purification. Herein, ruthenium doped carbon nitride (CNRu) was synthesized via a facile one-pot method, and CNRu was in form of Ru–N 2 that could efficiently activate PMS for DCF degradation and detoxification via nonradical pathway. DCF was completely removed within 10 min under the optimized condition in a wide working pH range of 3.00–9.00, while other traditional transition metals (e.g. Fe, Co, Ni, Cu) doped CN showed negligible removal of DCF due to adsorption rather than activation of PMS, which was demonstrated by DFT calculations. CNRu showed high stability and reusability after seven cycles and very few Ru leaching was detected in DCF degradation process. Ru was highly dispersed in form of Ru–N bond via coordinating to pyridine nitrogen, and the electron defect transfer between Ru and coordinated N, rather than redox cycle of Ru, mediated superoxide radicals (O 2 •− ) evolution, which was further hydrolyzed into singlet oxygen ( 1 O 2 ) and responsible for DCF removal. Thus, the CNRu/PMS system showed high tolerance to inorganic anions. Much lower toxic intermediates/products than DCF were obtained via the strong electrophilic attack reaction between 1 O 2 and DCF in CNRu/PMS system. This study displayed a new practical application prospect of ruthenium-based materials for high-efficient removal and detoxification of DCF from wastewater.

研究领域: 环境科学 · 催化材料 · 水处理技术
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PHARMAZIE · 2014 ·Vol. 69 ·期 12 ·898-903 · IF 1.003

The role of CYP2C9 genetic polymorphisms in the oxidative metabolism of diclofenac in vitro

Xia Meng-Ming,Wang Li,Pan Pei-Pei,Wang Hai-Yun,Chen Meng-Chun,Chen Yi,Dai Da-Peng,Cai Jian-Ping,Hu Guo-Xin

CYP2C9 is one of four known members of the human cytochrome P450 CYP2C superfamily, with at least 57 CYP2C9 alleles being previously identified. Genetic polymorphisms of CYP2C9 significantly influence the efficacy and safety of some drugs, which might cause adverse effects and therapeutic failure. The purpose of the present study was to clarify the role of 36 CYP2C9 alleles, 21 novel alleles (*36-*56) found in the Chinese population, in the oxidative metabolism of diclofenac in vitro. Insect microsomes expressing the 36 human CYP2C9 alleles were incubated with 2-100 μM diclofenac for 30 min at 37°C and terminated by the addition of 30 μL 0.1 M HCl. Diclofenac and 4'-hydroxyl (OH)-diclofenac, the major diclofenac metabolite, were analyzed by high-performance liquid chromatography (HPLC). Compared with wild-type CYP2C9*1, most variants showed significantly altered values in Vmax, Km and intrinsic clearance (Vmax/Km). Only one variant exhibited markedly increased intrinsic clearance value, whereas 31 variants exhibited significantly decreased values. Thus, this study demonstrated that more attention should be given to subjects carrying these CYP2C9 alleles when administering diclofena.

CAS / MDL: 7647-01-0
研究领域: 药理学 · 遗传学
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ELECTROANALYSIS · 2015 ·Vol. 28 ·期 1 ·76-82 · IF 2.138

Simultaneous Electrochemical Determination of Paracetamol and Diclofenac Based on Poly(diallyldimethylammonium chloride) Functionalized Graphene

Otieno Kevin Okoth,Kai Yan,Lan Liu,Jingdong Zhang

A simple but sensitive electrochemical method was proposed for simultaneous determination of paracetamol (PCT) and diclofenac (DCF) based on poly(diallyldimethylammonium chloride) (PDDA) functionalized graphene (GR). Although GR enhanced the electro-oxidation peak currents of PCT and DCF, the peak potential difference between two drugs was reduced. By contrast, PDDA-GR greatly increased the electrochemical currents of both analytes while provided well-separated peak potentials. Thus, the voltammetric behavior and simultaneous electrochemical determination of PCT and DCF were investigated on PDDA-GR. The applicability of the proposed method was verified when it was applied in determination of PCT and DCF in pharmaceuticals and lake water.

CAS / MDL: 26062-79-3
研究领域: 分析化学 · 药物分析 · 材料科学
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CHEMOSPHERE · 2021 · IF 7.086

Removal of diclofenac and oxytetracycline from synthetic urine by furfuryl alcohol-derived mesoporous carbon

Xiaoyi Xu,Zhimin He,Hui Tang,Yidong Sun,Shuyuan Zhang,Dezhi Shi,Fangying Ji

In this study, using furfuryl alcohol as the precursor carbon and mesoporous silica as the template, and furfuryl alcohol-derived mesoporous carbon (FMC) was prepared. The specific surface area of FMC was 1022.61 m 2 /g, the pore volume was 1.71 cm 3 /g, and the mesoporous volume was 98.8%. Based on the adsorption kinetics of pharmaceuticals onto the FMC in synthetic urine, equilibrium adsorption was reached in 120 min, and it followed a pseudo-second-order model. The adsorption isotherms were well-fitted by the Sips isotherm model, and the saturated adsorption capacities of diclofenac and oxytetracycline in fresh urine were 411.8 mg/g and 465.9 mg/g, respectively. Batch experiment results showed that pharmaceutical removal was strongly influenced by urine components such as sodium chloride, urea, and ammonium hydroxide. The adsorption of diclofenac and oxytetracycline was influenced by many factors including π-π interactions, hydrogen bonds , and electrostatic forces. FMC exhibited excellent reusability and retained urine nutrients during pharmaceutical adsorption.

CAS / MDL: 15307-79-6 2058-46-0
研究领域: 环境科学 · 材料科学
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH · 2022 ·Vol. 30 ·期 5 ·11959-11977 · IF 5.19

The efficient degradation of diclofenac by ferrate and peroxymonosulfate: performances, mechanisms, and toxicity assessment

He Haonan,Zhao Junfeng

In this study, the degradation efficiency and reaction mechanisms of diclofenac (DCF), a nonsteroidal anti-inflammatory drug, by the combination of ferrate (Fe(VI) and peroxymonosulfate (PMS) (Fe(VI)/PMS) were systematically investigated. The higher degradation efficiency of DCF in Fe(VI)/PMS system can be obtained than that in alone persulfate (PS), Fe(VI), PMS, or the Fe(VI)/PS process at pH 6.0. DCF was efficiently removed in Fe(VI)/PMS process within a wide range of pH values from 4.0 to 8.0, with higher degradation efficiency in acidic conditions. The increasing reaction temperature (10 to 30 ℃), Fe(VI) dose (6.25 to 100 µM), or PMS concentration (50 to 1000 µM) significantly enhanced the DCF degradation. The existences of HCO 3 ¯, Cl¯, and humic acid (HA) obviously inhibited the DCF removal. Electron paramagnetic resonance (EPR), free radical quenching, and probing experiments confirmed the existence of sulfate radicals (SO 4 • ¯), hydroxyl radicals ( • OH), and Fe(V)/ Fe(IV), which are responsible for DCF degradation in Fe(VI)/PMS system. The variations of TOC removal ratio reveal that the adsorption of organics with ferric particles, formed in the reduction of Fe(VI), also were functioned in the removal process. Sixteen DCF transformation byproducts were identified by UPLC-QTOF/MS, and the toxicity variation was evaluated. Consequently, eight reaction pathways for DCF degradation were proposed. This study provides theoretical basis for the utilization of Fe(VI)/PMS process. Graphical abstract

研究领域: 环境科学 · 化学工程
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF COLLOID AND INTERFACE SCIENCE · 2016 · IF 3.782

Interfacial thermodynamics and kinetics of sorption of diclofenac on prepared high performance flower-like MoS2

Yalei Zhang,Zengfu Yin,Chaomeng Dai,Xuefei Zhou,Wen Chen

Flower-like MoS 2 with numerous wrinkled nanosheets was prepared via a facile hydrothermal method . The surface morphology and microstructure of the obtained materials were characterized using X-ray diffraction data (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Additionally, the compositions of the flower-like MoS 2 were further revealed by an energy dispersion spectrometer (EDX) and X-ray photoelectron spectrometry (XPS). The obtained MoS 2 was used as an adsorbent to remove diclofenac (DCF, C 14 H 10 Cl 2 NO 2 Na) from aqueous solutions and presented excellent performance for removing DCF. The sorption kinetics, isotherms and effect of solution pH on the sorption were evaluated in batch sorption experiments. The sorption characteristics of the interactions between DCF and MoS 2 in water were analyzed using a pseudo-second-order model, an intraparticle diffusion model and Boyd model to determine the sorption rate-determining steps. It was concluded that the sorption of DCF on MoS 2 was fitted better by the pseudo-second-order model and that external diffusion governed the sorption process of DCF onto the MoS 2 . The interfacial interaction free energies between DCF and MoS 2 in the sorption process can be calculated based on the extended Derjaguin–Landau–Verwey–Overbeek (XDLVO). The flower-like MoS 2 presenting excellent performance for removing DCF, could be a better choice of treating DCF-containing wastewaters.

研究领域: 环境科学 · 材料科学
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ENVIRONMENTAL POLLUTION · 2021 · IF 8.071

Electro/magnetic superposition effects on diclofenac degradation: Removal performance, kinetics, community structure and synergistic mechanism

Yan Feng,Zichen Li,Yingying Long,Ning Suo,Zhongwei Wang,Lipin Qiu

Electric and magnetic fields characterized by high efficiency, low consumption and environment-friendly performance have recently generated interest as a possible measure to enhance the performance of the biological treatment process used to remove refractory organics. Few studies have been carried out to-date regarding the simultaneous application of electric and magnetic fields on biofilm process to degrade diclofenac. In this study, 3DEM-BAF was designed to evaluate the electrio-magnetic superposition effect on diclofenac removal performance, kinetics, community structure and synergistic mechanism. The results show that 3DEM-BAF could significantly increase the average removal rate of diclofenac by 65.30 %, 57.46 %, 9.48 % as compared with that of BAF, 3DM-BAF, 3DE-BAF, respectively. The diclofenac degradation kinetic constants and dehydrogenase activity of 3DEM-BAF were almost 6.72 and 2.53 times higher than those of BAF. Microorganisms of 3DEM-BAF in the Methylophilus and Methyloversatilis genera were distinctively enriched, which was attributed to the screening function of electric field and propagation effect of magnetic field. Moreover, three processes were found to contribute to diclofenac degradation, namely electro-magnetic-adsorption, electro-chemical oxidation and electro-magnetic-biodegradation. Thus, the simultaneous application of electric and magnetic fields on biofilm process was demonstrated to be a promising technique as well as a viable alternative in diclofenac degradation enhancement.

研究领域: 环境科学 · 微生物学
✓ 已验证 DOI 高影响因子
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ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY · 2017 · IF 3.743

Degradation of diclofenac by UV-activated persulfate process: Kinetic studies, degradation pathways and toxicity assessments

Xian Lu,Yisheng Shao,Naiyun Gao,Juxiang Chen,Yansen Zhang,Huiming Xiang,Youluo Guo

Diclofenac (DCF) is the frequently detected non-steroidal pharmaceuticals in the aquatic environment. In this study, the degradation of DCF was evaluated by UV-254   nm activated persulfate (UV/PS). The degradation of DCF followed the pseudo first-order kinetics pattern. The degradation rate constant (k obs ) was accelerated by UV/PS compared to UV alone and PS alone. Increasing the initial PS dosage or solution pH significantly enhanced the degradation efficiency. Presence of various natural water constituents had different effects on DCF degradation, with an enhancement or inhibition in the presence of inorganic anions (HCO 3 − or Cl − ) and a significant inhibition in the presence of NOM. In addition, preliminary degradation mechanisms and major products were elucidated using LC-MS/MS. Hydroxylation, decarbonylation, ring-opening and cyclation reaction involving the attack of SO 4 • − or other substances, were the main degradation mechanism. TOC analyzer and Microtox bioassay were employed to evaluate the mineralization and cytotoxicity of solutions treated by UV/PS at different times, respectively. Limited elimination of TOC (32%) was observed during the mineralization of DCF. More toxic degradation products and their related intermediate species were formed, and the UV/PS process was suitable for removing the toxicity. Of note, longer degradation time may be considered for the final toxicity removal.

研究领域: 环境科学 · 化学工程 · 毒理学
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DRUG DELIVERY · 2014 · IF 2.202

Cationic polymer-based micro-emulgel with self-preserving ability for transdermal delivery of diclofenac sodium

Chunyu Yang,Yan Shen,Jue Wang,Ammar Ouahab,Tao Zhang,Jiasheng Tu

The objective of the present study was to develop a topical preparation with enhanced skin permeation, high safety and self-preserving ability. Microemulsion (ME) and cationic polymer based micro-emulgel (CPBM) were investigated for the transdermal delivery of diclofenac sodium (DS). Medium-chain triglyceride was selected as the oil phase of ME due to its good solubilization of DS and high safety. Orthogonal test was applied to optimize the formula of ME based on the cumulative skin permeation amount in vitro after preliminary formula test. Chitosan (CS) or polylysine was employed as the cationic polymer in the formula of CPBM. The transdermal delivery of DS was evaluated through in vitro skin permeation test. The results showed that the skin permeation rate of DS from the optimized CPBM (126.17 ± 15.82 μg/cm2/h) were 1.86-folds and 5.76-folds higher than that of DS commercial Emulgel and DS control hydrogel, respectively. MEs and the cationic polymer were found to have skin penetration co-enhancing effect when they were combined in the CPBM system. Furthermore, the CPBM showed a good growth inhibition of E. coli and S. aureus. The stability test revealed that the CPBM was stable at room temperature and 4 °C for a period of three months.

研究领域: 药剂学 · 药物递送系统 · 皮肤科学
✓ 已验证 DOI 高影响因子
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CHEMOSPHERE · 2018 · IF 4.427

Degradation of diclofenac by H2O2 activated with pre-magnetization Fe0: Influencing factors and degradation pathways

Xiang Li,Minghua Zhou,Yuwei Pan

Diclofenac sodium (DCF) is frequently detected as a non-steroidal pharmaceutical in the aquatic environment. In this study, the degradation of DCF in two heterogeneous systems, pre-magnetization Fe 0 /H 2 O 2 (Pre-Fe 0 /H 2 O 2 ) and Fe 0 /H 2 O 2 system, was comparably studied. Our findings proved that Pre-Fe 0 could significantly improve the degradation and dechlorination of DCF due to the change of Fe 0 characteristics after pre-magnetization. Compared with Fe 0 /H 2 O 2 process, Pre-Fe 0 /H 2 O 2 process has 2.1–7.0 times higher rate constant for DCF degradation at different H 2 O 2 dosages (0.25–2.0 mM), initial pH (3.0–6.0) and Fe 0 dosages (0.25–1.5 mM). The characterizations by X-ray Photoelectron Spectroscopy and Electron Paramagnetic Resonance confirmed that the enhancement attributed to the increase of Fe 0 corrosion and fast generation of OH . In addition, preliminary degradation mechanism was elucidated by major products identification using UPLC-MS, through which the degradation intermediates, such as 4-hydroxy-diclofenac or 5-hydroxydiclofenac, 2,6-dichloroaniline, phenylacetic acid, 1,3-dichlorobenzene and 2-aminophenylacetic acid were identified. Hydroxylation, decarboxylation , C N bond cleavage and ring-opening involving the attack of OH or other substances, were the main degradation mechanism. Therefore, Pre-Fe 0 /H 2 O 2 process, which does not need extra energy and costly reagents, is an efficient and environmental-friendly process to degrade DCF.

研究领域: 环境科学 · 化学工程
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