Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 6
·511-520
·
IF 0.6
Zhang Mengmeng,Zou Qiaogen
Background: Atopic dermatitis (AD) is an allergic skin disease that can be inherited. Crisaborole is a specific drug developed to deal with this disease. The compounds of 4-(4- Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4-bromo-3-formylphenoxy)-3- formylphenoxy) benzonitrile
are the representative impurities in the synthesis of Crisaborole active pharmaceutical in gradient (API). Owing to the genotoxic impurities that could lead to cancer and gene mutations, it is necessary to develop a simple, efficient, sensitive, and accurate method to detect these impurities.
In this study, the 4-(4-Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4- bromo-3-formylphenoxy)-3-formylphenoxy)benzo- nitrile present in Crisaborole API were detected using UPLC-MS/MS. Methods: The separation was made on a ZORBAX Eclipse XDB-Pheny column (4.6 mm ×75mm, 3.5
μm) with the mobile phase of acetonitrile solution containing 0.1% trifluoroacetic acid (A) and water containing 0.1% formic acid (B) in gradient elution mode. Quantification was performed using positive ion electrospray ionization (ESI), and the contents of two compounds were determined
using the multiple reaction monitoring (MRM) modes. Results: The quantitative analytical method was fully validated with respect to linearity (r > 0.9998), sensitivity, precision, accuracy (the average recovery of two impurities was 84.1% to 90.7%), and robustness. Conclusion:
Three batches of samples were detected by UPLC-MS/MS, indicating that the proposed approach was applicable for the quality evaluation of Crisaborole.
研究领域:
药物分析
·
皮肤病学
·
毒理学
✓ 已验证
DOI
高影响因子
TALANTA
·
2021
·
IF 6.057
Qian Wang,Huanshun Yin,Jia Ding,Xi Fang,Yunlei Zhou,Shiyun Ai
The endogenous epigenetic marker 5-formylcytosine (5 fC) is introduced by 5-methylcytosine (5 mC) oxidation under action of enzyme oxidation, and plays an important role in many life activities. Since the content of 5 fC in mammalian tissues and cells is very low, it is necessary to exploit a sensitive and specific detection method to further understand the function of 5 fC. In this work, a sensitively and selectively photoelectrochemical (PEC) biosensor was developed for 5-formyl-2′-deoxycytidine (5fdC) detection. CuBi 2 O 4 /ZnPc@WS 2 was used as photoactive material, where the formed ternary heterojunction structure greatly enhanced the PEC response and increased the detection sensitivity. Positively charged polyethyleneimine (PEI) was employed as 5fdC recognition and capture unit, where the amine group on PEI specifically reacted with aldehyde group of 5fdC to form stable amide bond. 4-Carboxyphenylboronic acid (4-CPBA) was adopted as crosslinker for 5fdC and amino functionalized CuBi 2 O 4 based on the covalent interaction between 1,3-diol bond on 5fdC and boric acid structure on 4-CPBA, and the covalent interaction between –COOH on 4-CPBA and –NH 2 on amino functionalized CuBi 2 O 4 . On the basis of the positive synergistic effect of ZnPc and CuBi 2 O 4 on improving the photoelectric performance of WS 2 , the separation of photo-generated electron-hole pairs in semiconductors were promoted, and the examination range was expanded from 0.1 to 500 nM, and the detection limit was 0.0483 nM (3σ). Based on the unique covalent reaction between –NH 2 and –CHO, the PEC biosensor has excellent detection sensitivity, and can even separate 5fdC from 5-methylcytosine deoxyribonucleoside and 5-hydroxymethylcytosine deoxyribonucleoside. The effect of antibiotics and heavy metals on the 5fdC content in wheat tissue genome has also been further investigated using this sensor.
研究领域:
分析化学
·
生物化学
·
材料科学
·
纳米技术
✓ 已验证
DOI
高影响因子
Molecular Medicine Reports
·
2019
·Vol. 20
·期 6
·5084-5090
·
IF 1.851
Jinsan Yang,Cao Ma,Maoshu Zhang
Diabetes mellitus adversely affects human bones and increases the risk of developing osteoporosis. In the present study, treatment with 30 mmol/l glucose was used to establish a high glucose (HG) cell model in vitro. Plasmids were used to overexpress the P2X purinoceptor 7 (P2X7) gene. Brilliant blue G and (4‑benzoyl‑benzoyl)‑ATP were used as a P2X7 antagonist and agonist, respectively. Proliferation of osteogenic MC3T3‑E1 cells and alkaline phosphatase (ALP) activity were determined using MTT and colorimetric assays, respectively. Alizarin Red S was used to assess calcification of MC3T3‑E1 cells. Western blotting and reverse transcription‑quantitative PCR were performed to determine protein and mRNA expression levels. The results demonstrated that HG inhibited MC3T3‑E1 cell proliferation and P2X7 expression, reduced calcification, and downregulated the expression levels of ALP and osteocalcin (Ocn) in MC3T3‑E1 cells. Overexpression of P2X7 in HG conditions increased calcification and proliferation, and upregulated the levels of ALP and Ocn in MC3T3‑E1 cells. Inhibition of P2X7 downregulated the expressions of ALP and Ocn in MC3T3‑E1 cells under HG conditions. Therefore, the present results indicated that HG caused damage to osteogenic MC3T3‑E1 cells. Thus, P2X7 may be a regulatory factor that may be used to counteract the effects of HG on osteogenesis.
研究领域:
内分泌学
·
细胞生物学
·
分子生物学
·
糖尿病研究
·
骨骼生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Xuejing Lou,Yingge Hao,Huina Zhou,Zhen Song,Youmei Wang,Minghua Lu
The creation of defects in crystalline structures can tune metal-organic frameworks (MOFs) properties, such as improving their adsorptive and catalytic performance with producing more porosity and active sites. In this work, the bimetallic UiO-66 containing Zn and Zr was prepared. And then UiO-66 with missing cluster defects (UiO-66-1/3) were obtained by acid washing to remove the Zn nodes. UiO-66-1/3 was used as sorbent of dispersive solid-phase extraction (dSPE) to extract and enrich (BUs). Combination with high-performance liquid chromatography-diode array detector (HPLC-DAD) was developed to detect trace BUs in soil samples. Adsorption equilibrium can be reached in 3 min. The method possesses high enrichment factor (202-325), low detection limit (0.005-0.04 ng·mL -1 ), and wide linear range (0.02-200 ng·mL -1 ). In addition, the recovery rate of UiO-66-1/3 as an adsorbent was still higher than 95% after reused for 16 times. This work provides a new material for the enrichment and detection of benzoylurea insecticides in the environment.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2021
·Vol. 45
·期 28
·12585-12592
·
IF 3.591
Shuwei Lin,Qiyun Tong,Pan Jiang,Baozong Li,Yi Li,Yonggang Yang
Three dipeptides based on the Ala–Ala building block with different substituent positions of the dodecyloxy group on the benzoyl residue at the N terminus were designed and synthesized (ortho-, meta- and para-16). All of them were able to spontaneously self-assemble in the mixed solvent of methanol and water (6/4, v/v). However, three dipeptides underwent a distinct kinetically controlled self-assembling process. The spectroscopic study also revealed that, for ortho-16, the phenylene groups and the peptide sequence loosely packed, while meta- and para-16 stacked into well-ordered structures with the formation of parallel β-sheets through supramolecular self-assembly. Intramolecular hydrogen bonding and steric hindrance of the dodecyloxy side chain were proposed to lead to the different self-assembling behaviour of the three isomers.
研究领域:
生物化学
·
超分子化学
✓ 已验证
产品关联
DOI
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2021
·Vol. 45
·期 36
·16482-16489
·
IF 3.591
Zhenzhen Yang,Bangchong Zhu,Yuhan He,Genlei Zhang,Peng Cui,Jianbo He
In this study, α-MoO3 nanobelts were successfully synthesized by a simple, green and economic hydrothermal method and applied as a bifunctional catalyst for one-step conversion of fructose to DFF under atmospheric air. The structure of the as-prepared α-MoO3 catalyst was characterized in detail by SEM, TEM, EDS, XRD, XPS, H2-TPR and NH3-TPD to better understand the relationship between structure and performance. α-MoO3 nanobelts exhibited high catalytic activities for production of DFF from HMF and fructose in atmospheric air. Under optimized reaction conditions, high DFF yields of 97.2% and 78.3% were obtained by using HMF and fructose as raw materials, respectively. Furthermore, a plausible reaction pathway was proposed for the selective oxidation of HMF to DFF according to the experimental and catalyst characterization results. Importantly, α-MoO3 is a robust catalyst that can be used at least five times without obvious loss in its catalytic activity. In brief, α-MoO3 is an easily-prepared, eco-friendly, low cost and highly effective catalyst which has potential application in one-step conversion of fructose to DFF under atmospheric air.
研究领域:
材料科学
·
催化化学
✓ 已验证
DOI
高影响因子
Catalysis Science & Technology
·
2022
·Vol. 12
·期 9
·2903-2911
·
IF 6.177
Zhenzhen Yang,Yuhan He,Pengfei Tang,Bangchong Zhu,Genlei Zhang,Jianbo He
Direct conversion of biomass-based fructose to 2,5-diformylfuran (DFF) has attracted much attention in recent years. In this study, molybdenum carbide anchored on glucose-derived carbon (β-Mo2C@C) was synthesized by a simple, green and economical method and was found to be highly active for production of DFF from 5-hydromethylfurfural (HMF) and fructose. DFF was obtained with high yields of 94.5% and 76.0% from aerobic oxidation of HMF and “one-pot” conversion of fructose under optimal reaction conditions, respectively. A probable mechanism involving Mo6+/Mo2+ redox cycles was proposed for β-Mo2C@C-catalyzed oxidation of HMF to DFF according to the experimental and characterization results. Furthermore, the β-Mo2C@C catalyst can be reused without much loss of catalytic activity, suggesting that β-Mo2C@C is highly stable.
研究领域:
化学工程
·
催化材料科学
✓ 已验证
DOI
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2024
·
IF 13.3
Xuan Gao,Zhihui Li,Shuxing Zhang,Dongsheng Zhang,Xinqiang Zhao,Baoquan Zhang,Yanji Wang
Developing cost-effective and inherently safe methods for accelerating the sustainable production of value-added chemicals from biomass presents a promising solution to the current energy crisis. This study introduces heterogeneous copper species anchored on a γ-Al 2 O 3 catalyst (Cu/γ-Al 2 O 3 ) with high dispersibility and small Cu particle size, synthesized via a straightforward incipient-wetness impregnation method. This method facilitates the selective anaerobic dehydrogenation of 5-hydroxymethylfurfural (HMF) into 2,5-diformylfuran (DFF) in the absence of any oxidant or hydrogen acceptor. An HMF conversion of 69.8 % and a DFF yield of 44.9 % were attained at 130 °C over a 12-h period. Extensive characterizations were conducted to elucidate the correlation between the catalyst’s structure and its dehydrogenation activity. The findings indicated that strong L-acid sites, elevated Cu dispersions, small Cu particle size and an increased number of Cu + active sites were conducive to enhanced dehydrogenation reactivity. The Cu/γ-Al 2 O 3 catalyst demonstrated superior catalytic efficiency and stability. A possible reaction mechanism is suggested, integrating DFT calculations with experimental observations. This research offers valuable insights into the selective conversion of HMF to DFF and encourages further exploration into the dehydrogenation of biomass alcohols into high-value chemicals under oxidant-free conditions.
研究领域:
化学工程
·
可再生资源与环境科学
✓ 已验证
产品关联
DOI
高影响因子
ENERGY & FUELS
·
2016
·
IF 2.835
Fan Wang,Liang Jiang,Junmei Wang,Zehui Zhang
In this study, the mesporous SBA-15 was prepared and used to graft biimidazole groups, which were used to anchor Ru3+ to give rise to a new ruthenium catalyst (SBA-15-Biimidazole-Ru). The structure of the SBA-15-Biimidazole-Ru catalyst was well characterized and used for the aerobic oxidation of 5-hydroxymethylfurfural (HMF) into 2,5-diformylfuran (DFF). Several important parameters were studied and found that the reaction solvent and oxygen pressure showed a crucial role in the activity of the as-prepared SBA-15-Biimidazole-Ru catalyst. HMF conversion of 96.9% and DFF yield of 88.7% were achieved after 11 h at 110 °C under 15 bar oxygen pressure. One important characteristic of the SBA-15-Biimidazole-Ru catalyst is that it was very stable without loss of its catalytic activity during the recycling experiments, which was due to the strong interaction between the Ru3+ and the Biimidazole groups on the surface of SBA-15. Finally, the direct conversion of fructose into DFF was also performed by the use of Amberlyst 15 and SBA-15-Biimidazole-Ru as two binary catalysts. The dehydration of fructose over Amberlyst 15 catalyst and the subsequent oxidation of HMF over SBA-15-Biimidazole-Ru catalyst afforded DFF with an overall yield of 72.4%.
研究领域:
化学工程
·
催化科学
✓ 已验证
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2022
·
IF 5.204
Xinyu Cui,Quan Wu,Jun Sun,Xiaoyu Gu,Hongfei Li,Sheng Zhang
A boron-based biological flame retardant phenylboronic acid functionalized chitosan (B-CH) was prepared by reacting chitosan (CH) with 4-formylphenylboronic acids. The structure characterization was carried out by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermogravimetric analysis. B-CH was added into polylactic acid (PLA) by the melt blending method to improve the fire performance of the composite. The results showed that the peak heat release rate (PHRR) of PLA-7% B-CH decreased to 432 kW·m −2 from 564 kW·m −2 of control PLA. The limiting oxygen index (LOI) was increased from 19.1% to 26.2%, and the vertical burning test (UL-94) could reach a V-0 rating. The B-CH participated in the char formation process, which could generate a continuous compact char layer during the combustion to effectively protect the PLA matrix. This work provided an effective strategy to develop environmental friendly flame retardant PLA composites.
研究领域:
材料科学
·
生物材料
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
Advanced Materials Interfaces
·
2023
·Vol. 10
·期 10
·2201882
·
IF 5.4
Jinbo Chen,Guangming Lu,Yu Hao,Yichao Lu,Liang-Feng Huang,Yajie Zhang
Highly efficient and eco-friendly antimicrobial agents are crucial to the development of future marine antifouling coatings. A high efficient and low bio-toxicity bio-based anti-biofoulant, 2,5-diformylfuran dioxime chelating with copper ions ( E -DFFD-Cu), is evaluated. Its minimal bactericidal concentration and the concentration for 50% of maximal effect (EC 50 ) are 4.95 and 7.03 µmol L −1 , respectively. Excellent anti-biofouling performance in marine environment in situ can be kept at least 90 days and with maximum release rate of copper ion of 0.01 µmol cm −2 d −1 . Alkyl radical (R·) and hydrogen radical (H·) derived from E -DFFD are enhanced via chelating copper(II) catalysis, which attracts and disrupts microbe cell membrane and pili between intimate cells, resulting in excellent anti-biofouling effect. This provides a new perspective for developing anti-biofoulant from anti-biofouling mechanism in the future.
研究领域:
海洋生物学
·
材料科学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
Polymer Chemistry
·
2013
·Vol. 5
·期 8
·2951-2960
·
IF 5.231
Minghui He,Guangxue Chen,Xun Huang,Ruixin Xu,Zhaohua Zeng,Jianwen Yang
N-Phthaloyltranexamic acid ammonium salt derivatives integrating with peroxides can invoke redox photopolymerization and propagating polymerization. A series of N-phthaloyltranexamic acid ammonium salt derivatives based on benzophenone, thioxanthen, and naphtha chromophores as novel photocaged bases were synthesized and characterized. In combination with a benzoyl peroxide initiator, these structures were able to initiate the amine-mediated redox photopolymerization of acrylates. In particular, the covalent binding of N-phthalimidoamino acid and type II chromophores (thioxanthone, benzophenone) improved remarkably the photoreactivity of photocaged bases (thioxanthen-DBU and benzophenone-DBU) compared to the parent compound. Furthermore, naphthal-DBU matches well the emission spectra of the mercury lamp with a dominant emission wavelength at 365 nm. More importantly, phthal-DBU & BPO as a new photocaged redox combination can invoke controlled redox polymerization within an irradiation time of 3 min. Finally, due to the persistent interaction of the produced longeval amine with peroxides, remarkable post conversion after irradiation, which is significant for preparation of photo-screened materials, was thus initially achieved in the redox photopolymerization.
研究领域:
材料化学
·
高分子科学
·
有机化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）